Slurry, polishing method, method for manufacturing component, and cerium oxide particles

A cerium oxide particle slurry with tailored properties addresses the challenge of high polishing speeds for insulating materials in 3D-NAND manufacturing, achieving efficient removal of insulating layers.

WO2026133463A1PCT designated stage Publication Date: 2026-06-25RESONAC CORP

Patent Information

Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
RESONAC CORP
Filing Date
2024-12-18
Publication Date
2026-06-25

AI Technical Summary

Technical Problem

Existing polishing technologies struggle to achieve high polishing speeds for insulating materials, particularly in the context of 3D-NAND device manufacturing where high step heights necessitate rapid removal of insulating material to maintain manufacturing throughput.

Method used

A slurry containing cerium oxide particles with specific properties, including a ratio of BET diameter to crystallite diameter on the (111) plane of 1.00 or more and integrated pore volume in the range of 0.11 to 0.17 cm², is used to enhance polishing speed and efficiency.

Benefits of technology

The slurry achieves high polishing speeds for insulating materials, such as silicon oxide, exceeding 2000 nm/min, by optimizing physical and chemical polishing performance through controlled particle properties.

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Abstract

Provided is a slurry containing abrasive grains and water, wherein the abrasive grains contain cerium oxide particles, the ratio of the BET diameter to the crystallite diameter in the (111) plane of the cerium oxide particles is 1.00 or more, and the integrated value of the differential pore volume distribution in the pore diameter range of 10-180 nm, is 0.11-0.17 cm3 / g in the pore distribution curve of the cerium oxide particles. This polishing method comprises a step for polishing a member to be polished using the slurry. Also provided is a method for manufacturing a component including a step of obtaining a component using the member to be polished polished with the polishing method.
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Description

Slurry, polishing method, part manufacturing method and cerium oxide particles

[0001] This disclosure relates to slurry, polishing methods, methods for manufacturing parts, and cerium oxide particles, etc.

[0002] In recent years, the importance of processing technologies for increasing density and miniaturization has been steadily growing in semiconductor device manufacturing processes. One such processing technology, CMP (chemical mechanical polishing), has become an essential technology in semiconductor device manufacturing processes for forming shallow trench isolation (STI), planarizing premetallic insulating materials or interlayer insulating materials, and forming plugs or embedded metal wiring.

[0003] The most commonly used polishing fluids include silica-based polishing fluids containing silica (silicon oxide) particles such as fumed silica and colloidal silica as abrasive grains. Silica-based polishing fluids are characterized by their versatility, and by appropriately selecting the abrasive grain content, pH, additives, etc., they can polish a wide range of materials, including both insulating and conductive materials.

[0004] On the other hand, there is a growing demand for cerium oxide-based polishing solutions containing cerium oxide particles as abrasives. For example, cerium oxide-based polishing solutions can polish insulating materials at high speed even with a lower abrasive content than silica-based polishing solutions (see, for example, Patent Documents 1 and 2 below).

[0005] JP-A-10-106994 JP-A-08-022970

[0006] Incidentally, in recent years, 3D-NAND devices, in which the cell portions of the device are stacked vertically, have been gaining prominence. In this technology, the step height of the insulating material during cell formation is several times higher compared to conventional planar type devices. Consequently, in order to maintain the throughput of device manufacturing, it is necessary to quickly eliminate the aforementioned high step height in the CMP process or other steps, and to improve the polishing speed of the insulating material.

[0007] One aspect of this disclosure aims to provide a slurry capable of achieving a high polishing speed for insulating materials. Another aspect of this disclosure aims to provide a polishing method using such a slurry. Another aspect of this disclosure aims to provide a method for manufacturing parts using such a polishing method. Another aspect of this disclosure aims to provide cerium oxide particles that can be used in such a slurry.

[0008] This disclosure relates, for example, to the following invention: [1] A solution containing abrasive grains and water, wherein the abrasive grains include cerium oxide particles, the ratio of the BET diameter to the crystallite diameter on the (111) plane of the cerium oxide particles is 1.00 or more, and the integrated value of the differential pore volume in the range of pore diameters from 10 to 180 nm in the pore distribution curve of the cerium oxide particles is 0.11 to 0.17 cm². 3 [1] A slurry that is 1 / g. [2] The slurry according to [1], wherein the BET diameter is 21.0 nm or more. [3] The slurry according to [1] or [2], wherein the crystallite diameter is 23.0 nm or less. [4] The slurry according to any one of [1] to [3], wherein the ratio is 1.70 or more. [5] The cumulative value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve is 0.12 to 0.21 cm 3 The slurry according to any one of [1] to [4], which is / g. [6] The cumulative value of the differential pore volume in the range of pore diameter 1.4 to 3.0 nm in the pore distribution curve is 0.0030 to 0.0065 cm 3[1] A slurry according to any one of [1] to [5], wherein the amount of abrasive grains is 0.01 to 10.00% by mass. [2] A slurry according to any one of [1] to [6], wherein the amount of abrasive grains is 0.01 to 10.00% by mass. [3] A slurry according to any one of [1] to [7], wherein the average particle size of the abrasive grains is 100 to 600 nm. [4] A slurry according to any one of [1] to [8], wherein the pH is 1.0 to 7.0. [5] A polishing method comprising the step of polishing a workpiece using a slurry according to any one of [1] to [9]. [6] A polishing method according to

[10] , wherein the workpiece contains silicon dioxide. [7] A method for manufacturing a part, comprising the step of obtaining a part using a workpiece polished by the polishing method according to

[10] or

[11] .

[13] The ratio of the BET diameter to the crystallite diameter on the (111) plane is 1.00 or greater, and the cumulative value of the differential pore volume in the pore diameter range of 10 to 180 nm on the pore distribution curve is 0.11 to 0.17 cm 3 Cerium oxide particles, weighing / g.

[0009] According to one aspect of this disclosure, a slurry capable of achieving a high polishing speed for insulating materials can be provided. According to another aspect of this disclosure, a polishing method using such a slurry can be provided. According to yet another aspect of this disclosure, a method for manufacturing parts using such a polishing method can be provided. According to yet another aspect of this disclosure, cerium oxide particles that can be used in such a slurry can be provided.

[0010] The embodiments of this disclosure will be described in detail below.

[0011] <Definitions> In this specification, numerical ranges indicated using "~" represent a range that includes the numbers listed before and after "~" as the minimum and maximum values, respectively. "A or greater" in a numerical range means A and the range greater than A. "A or less" in a numerical range means A and the range less than A. In numerical ranges described stepwise in this specification, the upper or lower limit of a numerical range in one step can be arbitrarily combined with the upper or lower limit of a numerical range in another step. In numerical ranges described in this specification, the upper or lower limit of that numerical range may be replaced with the values ​​shown in the examples. "A or B" means that either A or B may be included, or both may be included. Unless otherwise specified, the materials exemplified in this specification can be used individually or in combination of two or more. The content of each component in a composition means the total amount of multiple substances present in the composition if there are multiple substances corresponding to each component in the composition, unless otherwise specified. The term "membrane" encompasses not only structures formed across the entire surface when observed in a plan view, but also structures formed only in parts of the surface. The term "process" includes not only independent processes, but also processes that cannot be clearly distinguished from other processes, as long as their intended function is achieved.

[0012] As will be described later, the slurry according to this embodiment contains abrasive grains. Abrasive grains are also called "abrasive particles," but in this specification they are referred to as "abrasive grains." Abrasive grains are generally solid particles, and it is thought that during polishing, the material to be removed is removed by the mechanical action of the abrasive grains and the chemical action of the abrasive grains (mainly the surface of the abrasive grains), but this is not limited to this.

[0013] <Slurry> The slurry according to this embodiment contains abrasive particles and water. The slurry according to this embodiment can be used, for example, as a polishing liquid (CMP polishing liquid). In this specification, "polishing liquid" is defined as a composition that comes into contact with the surface to be polished during polishing. The term "polishing liquid" itself does not limit the components contained in the polishing liquid in any way.

[0014] In the slurry according to this embodiment, the abrasive grains include cerium oxide particles, the ratio of the BET diameter to the crystallite diameter (crystallite diameter / BET diameter) on the (111) plane of the cerium oxide particles is 1.00 or more, and the integrated value of the differential pore volume in the range of pore diameters from 1.4 to 180 nm in the pore distribution curve of the cerium oxide particles is 0.11 to 0.17 cm². 3 It is / g.

[0015] According to the slurry of this embodiment, it is possible to obtain a high polishing speed for insulating materials, for example, a high polishing speed for silicon oxide, and a high polishing speed for silicon oxide derived from TEOS (tetraethoxysilane) (silicon oxide obtained using TEOS) can be obtained. According to the slurry of this embodiment, in the evaluation method described in the examples below, a polishing speed of 20 seconds of polishing of insulating material (silicon oxide) can be obtained, for example, 2000 nm / min or more (preferably 2050 nm / min or more, 2100 nm / min or more, 2150 nm / min or more, etc.).

[0016] The factors that enable high polishing speeds for insulating materials are not entirely clear, but they are presumed to be as follows. However, the factors are not limited to those listed below. Specifically, the crystallite size at the (111) plane of cerium oxide particles is an indicator of the number of grain boundaries in the particles. The smaller the crystallite size, the more grain boundaries there are, and the more easily the particles break as polishing progresses, thus exposing new crystal planes with high reactivity (high chemical reactivity). On the other hand, the BET diameter is an indicator of particle density. The larger the BET diameter, the denser the cerium oxide particles become, resulting in higher physical polishing performance. Therefore, when the ratio of the BET diameter to the crystallite size at the (111) plane is relatively large, both physical and chemical polishing performance tend to be superior. Furthermore, the cumulative value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve of cerium oxide particles can be considered as the pore volume of pores with a diameter of 1.4 to 180 nm. Since pores with a diameter of 1.4 to 180 nm are thought to represent pores between cerium oxide particles, it can be said that the aggregation of cerium oxide particles is suppressed because this cumulative value is relatively large. As a result, there are more reaction sites on the surface of the cerium oxide particles, and the chemical polishing performance is improved. Therefore, it is presumed that a slurry containing such cerium oxide particles has sufficiently high physical and chemical polishing performance, and can obtain a high polishing rate for insulating materials.

[0017] This embodiment provides a method for adjusting the polishing speed, which adjusts the polishing speed based on the ratio of the BET diameter to the crystallite diameter in the (111) plane of cerium oxide particles, and the integrated value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore diameter range of the pore distribution curve. This embodiment also provides a method for selecting abrasive grains, which selects abrasive grains containing cerium oxide particles based on the ratio of the BET diameter to the crystallite diameter in the (111) plane, and the integrated value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve. This embodiment also provides the use of slurry for polishing surfaces containing insulating materials, and for polishing surfaces containing silicon oxide. This embodiment also provides the use of slurry in the planarization process of a substrate surface, which is a semiconductor device manufacturing technology. This embodiment also provides the use of slurry in the planarization process of STI insulating materials, premetal insulating materials, or interlayer insulating materials.

[0018] (Abrasive grains) The slurry according to this embodiment contains abrasive grains, which include cerium oxide particles (particles containing cerium oxide). The cerium oxide in the cerium oxide particles may contain tetravalent cerium or trivalent cerium. The cerium oxide particles may contain metal elements other than cerium, or they may not contain metal elements other than cerium. The content of metal elements other than cerium in the cerium oxide particles may be less than 1 mol% based on the total mass of the cerium oxide particles. Examples of metal elements include alkaline earth metals such as beryllium, magnesium, calcium, strontium, barium, and radium; and lanthanides such as lanthanum, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, and lutetium.

[0019] The abrasive grains may contain particles other than cerium oxide particles. Examples of particles other than cerium oxide particles include silicon oxide (silica) particles, aluminum oxide (alumina) particles, silicon nitride particles, zirconium oxide (zirconia: yttria-doped zirconia particles, etc.) particles, titanium oxide (titania) particles, yttrium oxide (yttria) particles, silicon carbide particles, diamond particles, polymer particles, and the like.

[0020] The cerium oxide (cerium oxide particles) content may be within the following ranges based on the total mass of abrasive grains (total mass of abrasive grains contained in the slurry): From the viewpoint of easily obtaining a high polishing speed for insulating materials, the cerium oxide (cerium oxide particles) content may be 20% by mass or more, 30% by mass or more, 40% by mass or more, 50% by mass or more, more than 50% by mass, 60% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 95% by mass or more, 98% by mass or more, or 99% by mass or more. The slurry may be configured such that the abrasive grains contained in it are substantially composed of cerium oxide (cerium oxide particles) (a configuration in which the cerium oxide (cerium oxide particles) content is substantially 100% by mass based on the total mass of abrasive grains contained in the slurry).

[0021] Cerium oxide particles (cerium oxide powder) can be obtained, for example, by oxidizing a cerium compound. Methods for oxidizing the cerium compound include calcination and oxidation with hydrogen peroxide, etc. Calcination is preferable from the viewpoint of easily obtaining a high polishing rate for insulating materials and easily suppressing the decrease in polishing rate as polishing progresses. Examples of cerium compounds include cerium carbonate, cerium nitrate, cerium sulfate, and cerium oxalate. From the viewpoint of easily obtaining a high polishing rate for insulating materials and easily suppressing the decrease in polishing rate as polishing progresses, the cerium compound may be cerium carbonate, and the cerium oxide particles may contain oxides derived from cerium carbonate.

[0022] Cerium carbonate, used to obtain cerium oxide particles, can be obtained from natural minerals using the following procedure. First, rare earth concentrates (bastnäsite concentrate, monazite concentrate, Chinese complex concentrate, etc.) are obtained by removing unwanted gangue from ores containing rare earth elements, including at least cerium, through ore dressing. Next, the rare earth concentrates are subjected to chemical treatment (alkaline decomposition, sulfuric acid decomposition, hydroxide fractional precipitation, etc.) to reduce insoluble components such as impurities, and then, if necessary, rare earth elements (neodymium, etc.) are reduced by solvent extraction to obtain a cerium-containing rare earth salt solution. Finally, cerium carbonate can be obtained by mixing this cerium-containing rare earth salt solution with sodium carbonate. For convenience, this method of producing cerium carbonate is defined as the "extraction method."

[0023] Other cerium salts (cerium nitrate, cerium sulfate, cerium oxalate, etc.) can be synthesized by changing the sodium carbonate used in the "extraction method" to another salt. For example, cerium nitrate (e.g., cerium(III) nitrate) can be obtained by mixing a cerium-containing rare earth salt solution with sodium nitrate. Cerium carbonate can be obtained by reacting an aqueous solution of a cerium salt with a solution of a precursor having a carbonyl group. For example, cerium carbonate can be precipitated by reacting an aqueous solution of cerium nitrate (e.g., cerium(III) nitrate) with a solution of a precursor having a carbonyl group at a temperature of 80 to 100°C. Urea can be used as a precursor having a carbonyl group. For convenience, this method for producing cerium carbonate is defined as the "carbonyl substitution method". In this embodiment, the method for producing cerium carbonate may be either the "extraction method" or the "carbonyl substitution method", or it may be the "carbonyl substitution method", from the viewpoint of easily obtaining a high polishing rate for insulating materials and easily suppressing the decrease in polishing rate as polishing progresses.

[0024] The firing temperature in the firing method may be 350°C or higher, 400°C or higher, or 430°C or higher, from the viewpoint of easily obtaining a high polishing rate for the insulating material. The firing temperature may be 450°C or higher, 500°C or higher, or 550°C or higher. The firing temperature may be 900°C or lower, 850°C or lower, 800°C or lower, 750°C or lower, 700°C or lower, 650°C or lower, 600°C or lower, or 550°C or lower, from the viewpoint of easily obtaining a high polishing rate for the insulating material. The firing temperature may be 500°C or lower, or 450°C or lower. From these perspectives, the firing temperature may be 350-900°C, 350-800°C, 350-700°C, 350-600°C, 350-550°C, 400-900°C, 400-800°C, 400-700°C, 400-600°C, or 400-550°C.

[0025] From the viewpoint of easily obtaining a high polishing rate for the insulating material, the firing time in the firing method may be 0.1 hours or more, 0.5 hours or more, 1.0 hour or more, 2.0 hours or more, or 3.0 hours or more. From the viewpoint of easily obtaining a high polishing rate for the insulating material, the firing time may be 10.0 hours or less, 8.0 hours or less, 6.0 hours or less, 5.0 hours or less, 4.0 hours or less, or 3.0 hours or less. From these viewpoints, the firing time may be 0.1 to 10.0 hours, 0.1 to 8.0 hours, 0.1 to 6.0 hours, 0.1 to 3.0 hours, 1.0 to 10.0 hours, 1.0 to 8.0 hours, 1.0 to 6.0 hours, or 1.0 to 3.0 hours. The firing time refers to the firing time from when the temperature reaches 400°C until cooling begins.

[0026] In the firing method, the heating rate (heating rate up to 400°C) is preferably 1.0°C / min or less, more preferably 0.8°C / min or less, and even more preferably 0.6°C / min or less. When the heating rate is 1.0°C / min or less, volatile components present in the cerium oxide particles are gradually released, making the surface of the cerium oxide particles less prone to roughening, and the BET specific surface area of ​​the cerium oxide particles tends to decrease (the BET diameter increases). In the firing method, the heating rate is preferably 0.1°C / min or more, more preferably 0.2°C / min or more, and even more preferably 0.3°C / min or more. When the heating rate is 0.1°C / min or more, firing can be completed in a short time, which suppresses the growth of crystallites of the cerium oxide particles and prevents the crystallite diameter of the cerium oxide particles from growing excessively large.

[0027] The atmospheric gas in the firing method may be air, oxygen, or an inert gas. From the viewpoint of easily obtaining a high polishing rate for the insulating material, it may be an inert gas or nitrogen. The oxygen concentration in the atmospheric gas in the firing method may be 50% by volume or less, 40% by volume or less, 30% by volume or less, 20% by volume or less, 10% by volume or less, or 5% by volume or less, from the viewpoint of easily obtaining a high polishing rate for the insulating material.

[0028] In the firing method, the average cooling rate is preferably 3.0°C / min or higher, more preferably 3.5°C / min or higher, and even more preferably 4.0°C / min or higher. The average cooling rate refers to the average value of the cooling rate from the start to the end of cooling. When the average cooling rate is 3.0°C / min or higher, the growth of crystallites of cerium oxide particles can be suppressed, and the crystallite diameter of cerium oxide particles can be prevented from growing excessively large. In the firing method, the average cooling rate is preferably 10.0°C / min or lower, more preferably 8.0°C / min or lower, and even more preferably 6.0°C / min or lower. When the average cooling rate is 10.0°C / min or lower, surface roughening of cerium oxide particles due to rapid temperature changes is suppressed, and the BET specific surface area of ​​cerium oxide particles tends to decrease (BET diameter increases).

[0029] Cooling in the firing method may be performed by air flow or natural cooling. Air flow can achieve a faster cooling rate than natural cooling.

[0030] For the cerium oxide particles obtained as described above, at least one treatment selected from the group consisting of grinding and classification may be performed so that cerium oxide particles having a specific range of particle sizes (for example, average particle size) can be obtained.

[0031] The BET specific surface area of the cerium oxide particles is 50.0 m 2 / g or less, 45.0 m 2 / g or less, 42.0 m 2 / g or less, 40.0 m 2 / g or less, or less than 40.0 m 2 / g may be. The BET specific surface area is 38.0 m 2 / g or less, 35.0 m 2 / g or less, 34.0 m 2 / g or less, 33.0 m 2 / g or less, 32.0 m 2 / g or less, 31.0 m 2 / g or less, 30.0 m 2 / g or less, 30.0 m 2 / g less than, or less than 29.0 m 2 / g may be. From the viewpoint that as the BET specific surface area of the cerium oxide particles increases, the number of reaction points on the surface of the cerium oxide particles increases, the chemical reactivity is likely to improve, and the polishing rate of the insulating material is likely to improve, 16.0 m 2 / g or more, 17.0 m 2 / g or more, 18.0 m 2 / g or more, 19.0 m 2 / g or more, 20.0 m 2 / g or more, 20.0 m 2 / g more than, more than 20.5 m 2 / g or more, 21.0 m 2 / g or more, 21.5 m 2 / g or more, 22.0 m 2 / g or more, 23.0 m 2 / g or more, 25.0m 2 / g or more, 27.0m 2 / g or more, or 28.0m 2 It may be greater than or equal to / g. The BET specific surface area is 29.0 m². 2 / g or more, 30.0m 2 / g or more, 31.0m 2 / g or more, 32.0m 2 / g or more, 33.0m 2 / g or more, 34.0m 2 / g or more, 35.0m 2 / g or more, 36.0m 2 / g or more, 37.0m 2 / g or more, 38.0m 2 / g or more, or 39.0m 2 It may be greater than or equal to / g. From these perspectives, the BET specific surface area is 16.0 to 50.0 m². 2 / g, 16.0-40.0m 2 / g, 16.0-35.0m 2 / g, 16.0-33.0m 2 / g, 19.0-50.0m 2 / g, 19.0-40.0m 2 / g, 19.0-35.0m 2 / g, 19.0-33.0m 2 / g, 20.5-50.0m 2 / g, 20.5-40.0m 2 / g, 20.5-35.0m 2 / g, or 20.5-33.0m 2 It may be / g. The BET specific surface area can be obtained by the method described in the examples below.

[0032] The BET diameter is calculated assuming that the primary particles of cerium oxide are spherical, and S N It can be calculated from the true density ρ of the cerium oxide particles. Specifically, it can be calculated using the following formula. The true density ρ of the cerium oxide particles can be measured by the method described in the examples below. BET diameter = 6 / (ρ × S N )

[0033] The BET diameter of the cerium oxide particles may be 10.0 nm or larger, 15.0 nm or larger, 18.0 nm or larger, 20.0 nm or larger, greater than 20.0 nm, or 21.0 nm or larger, from the viewpoint of easily increasing the physical strength of the cerium oxide particles and easily improving the polishing speed of the insulating material. The BET diameter may be 22.0 nm or larger, 24.0 nm or larger, 25.0 nm or larger, 26.0 nm or larger, 27.0 nm or larger, 28.0 nm or larger, or 29.0 nm or larger. The BET diameter may be 50.0 nm or less, less than 50.0 nm, 49.0 nm or less, 48.0 nm or less, 46.0 nm or less, 44.0 nm or less, 42.0 nm or less, 40.0 nm or less, 39.0 nm or less, 38.5 nm or less, 38.0 nm or less, 37.0 nm or less, 35.0 nm or less, 33.0 nm or less, 31.0 nm or less, 30.0 nm or less, or less than 30.0 nm, from the viewpoint of easily improving the chemical reactivity of cerium oxide particles and easily improving the polishing speed of the insulating material. The BET diameter may be 29.0 nm or less, 28.0 nm or less, 27.0 nm or less, 26.0 nm or less, 25.0 nm or less, 24.0 nm or less, 23.0 nm or less, or 22.0 nm or less. From these perspectives, the BET diameter may be 10.0–50.0 nm, 10.0–44.0 nm, 10.0–40.0 nm, 10.0–38.5 nm, 10.0–33.0 nm, 10.0–30.0 nm, 20.0–50.0 nm, 20.0–44.0 nm, 20.0–40.0 nm, 20.0–38.5 nm, 20.0–33.0 nm, 24.0–30.0 nm, 24.0–50.0 nm, 24.0–44.0 nm, 24.0–40.0 nm, 24.0–38.5 nm, 24.0–33.0 nm, or 24.0–30.0 nm.

[0034] The crystallite size of the cerium oxide particles in the (111) plane may be 40.0 nm or less, 38.0 nm or less, 36.0 nm or less, 35.0 nm or less, less than 35.0 nm, 34.0 nm, 33.0 nm or less, 32.0 nm or less, 31.0 nm or less, 30.0 nm or less, less than 30.0 nm, 29.0 nm or less, 28.0 nm or less, 27.0 nm or less, 25.0 nm or less, 23.0 nm or less, 22.0 nm or less, or 21.0 nm or less, from the viewpoint of easily improving the chemical reactivity of the cerium oxide particles and easily improving the polishing speed of the insulating material. The crystallite size may be 20.0 nm or less, less than 20.0 nm, 19.0 nm or less, 18.0 nm or less, 17.0 nm or less, 15.0 nm or less, 14.0 nm or less, or 13.0 nm or less. The crystallite size may be 10.0 nm or larger, or 12.0 nm or larger, from the viewpoint of increasing the physical strength of the cerium oxide particles and improving the polishing speed of the insulating material. The crystallite size may be 13.0 nm or larger, 14.0 nm or larger, 15.0 nm or larger, 16.0 nm or larger, 17.0 nm or larger, 18.0 nm or larger, 19.0 nm or larger, 20.0 nm or larger, or greater than 20.0 nm. From these perspectives, the crystallite size may be 10.0–40.0 nm, 10.0–35.0 nm, 10.0–32.0 nm, 10.0–27.0 nm, 10.0–25.0 nm, 10.0–22.0 nm, 10.0–18.0 nm, 12.0–40.0 nm, 12.0–35.0 nm, 12.0–32.0 nm, 12.0–27.0 nm, 12.0–25.0 nm, 12.0–22.0 nm, 12.0–18.0 nm, 15.0–40.0 nm, 15.0–35.0 nm, 15.0–32.0 nm, 15.0–27.0 nm, 15.0–25.0 nm, 15.0–22.0 nm, or 15.0–18.0 nm.

[0035] The crystallite size can be derived by applying the Williamson-Hall method to data obtained from powder X-ray diffraction (XRD) of cerium oxide particles. In the Williamson-Hall method, sinθ is plotted on the x-axis and βcosθ (β = integral width) on the y-axis for all peaks of the X-ray diffraction pattern (XRD chart) obtained from XRD. A linear approximation line is created for the plotted points using the least squares method, and the crystallite size is obtained from the intercept of the approximation line. Commercially available XRD analysis software can be used; for example, the crystallite size can be derived using "PDXL2" manufactured by Rigaku Corporation. Specifically, the crystallite size can be obtained by the method described in the examples below.

[0036] The ratio of the BET diameter to the crystallite diameter on the (111) plane of the cerium oxide particles is 1.00 or higher, from the viewpoint of obtaining a high polishing rate for the insulating material. This ratio may be 1.05 or higher, 1.10 or higher, 1.12 or higher, 1.14 or higher, 1.15 or higher, 1.16 or higher, 1.17 or higher, 1.18 or higher, 1.19 or higher, or 1.20 or higher, from the viewpoint of having better physical and chemical polishing performance of the cerium oxide particles and easily improving the polishing rate of the insulating material. The ratio may be 1.22 or higher, 1.24 or higher, 1.26 or higher, 1.28 or higher, 1.29 or higher, 1.30 or higher, 1.32 or higher, 1.34 or higher, 1.35 or higher, greater than 1.35, 1.36 or higher, 1.37 or higher, 1.38 or higher, 1.40 or higher, 1.42 or higher, 1.43 or higher, 1.50 or higher, 1.60 or higher, 1.70 or higher, 1.80 or higher, 1.90 or higher, 2.00 or higher, greater than 2.00, 2.10 or higher, 2.12 or higher, 2.13 or higher, 2.14 or higher, or 2.15 or higher. The ratio may be 10.00 or less, 8.00 or less, 6.00 or less, 5.00 or less, 4.00 or less, 3.00 or less, 2.50 or less, 2.40 or less, 2.35 or less, 2.30 or less, 2.25 or less, 2.20 or less, 2.18 or less, 2.17 or less, 2.16 or less, or 2.15 or less, from the viewpoint of achieving superior physical and chemical polishing performance of cerium oxide particles and improving the polishing speed of insulating materials. The ratio may be 2.10 or less, 2.00 or less, 1.90 or less, 1.80 or less, 1.70 or less, 1.60 or less, 1.50 or less, 1.45 or less, 1.40 or less, less than 1.40, 1.38 or less, 1.37 or less, 1.36 or less, 1.35 or less, less than 1.35, 1.34 or less, 1.32 or less, 1.30 or less, 1.29 or less, less than 1.29, 1.28 or less, 1.26 or less, 1.25 or less, 1.24 or less, 1.23 or less, 1.22 or less, 1.21 or less, or 1.20 or less.From these perspectives, the ratios are 1.00-10.00, 1.00-2.50, 1.00-2.20, 1.00-2.00, 1.00-1.50, 1.00-1.40, 1.00 or more and less than 1.35, 1.00-1.30, 1.00-1.20, 1.10-10.00, 1.10-2.50, 1.10-2.20, 1.10-2.00, 1.10-1.50, 1.10-1.40, 1.10 or more and less than 1.35, 1.10-1.30, 1.10-1.20, and 1.20-10. It may be 00, 1.20-2.50, 1.20-2.20, 1.20-2.00, 1.20-1.50, 1.20-1.40, 1.20 or more and less than 1.35, 1.20-1.30, 1.30-10.00, 1.30-2.50, 1.30-2.20, 1.30-2.00, 1.30-1.50, 1.30-1.40, 1.30 or more and less than 1.35, 1.40-10.00, 1.40-2.50, 1.40-2.20, 1.40-2.00, or 1.40-1.50.

[0037] Based on the BJH method, a pore distribution curve can be obtained from the adsorption isotherm when nitrogen is used as the adsorption medium, with the horizontal axis representing pore diameter and the vertical axis representing differential pore volume. Specifically, the pore distribution curve can be obtained by the method described in the examples below.

[0038] The integrated value of the differential pore volume in the pore diameter range of 1.4–3.0 nm in the pore distribution curve of cerium oxide particles can be considered as the pore volume of pores with a diameter of 1.4–3.0 nm, and pores with a diameter of 1.4–3.0 nm are considered to represent pores within the cerium oxide particles. The integrated value of the differential pore volume in the pore diameter range of 1.4–3.0 nm in the pore distribution curve tends to have fewer pores in the cerium oxide particles, which increases the physical strength of the cerium oxide particles and improves the polishing speed of the insulating material, is 0.0080 cm². 3 / g or less, 0.0080cm 3 Less than 0.0075 cm / g 3 / g or less, 0.0070cm 3 / g or less, 0.0070cm 3 Less than 0.0068 cm / g 3 / g or less, 0.0066cm 3 / g or less, 0.0065cm3 / g or less, or 0.0064 cm 3 / g or less. The integrated value of the differential pore volume in the pore diameter range of 1.4 to 3.0 nm in the pore size distribution curve is 0.0062 cm 3 / g or less, 0.0060 cm 3 / g or less, 0.0060 cm 3 / g less than, 0.0058 cm 3 / g or less, 0.0056 cm 3 / g or less, 0.0055 cm 3 / g or less, 0.0054 cm 3 / g or less, 0.0052 cm 3 / g or less, 0.0050 cm 3 / g or less, 0.0050 cm 3 / g less than, 0.0048 cm 3 / g or less, 0.0046 cm 3 / g or less, 0.0045 cm 3 / g or less, 0.0044 cm 3 / g or less, 0.0042 cm 3 / g or less, 0.0040 cm 3 / g or less, 0.0040 cm 3 / g less than, or 0.0038 cm 3 / g or less. The integrated value of the differential pore volume in the pore diameter range of 1.4 to 3.0 nm in the pore size distribution curve tends to increase the surface area of the cerium oxide particles, and the chemical reactivity is likely to be improved due to the increase in the reaction points on the surface of the cerium oxide particles. From the perspective that the polishing rate of the insulating material is likely to be improved, 0.0010 cm 3 / g or more, 0.0015 cm 3 / g or more, 0.0020 cm 3 / g or more, 0.0020 cm 3 / g more than, 0.0025 cm 3 / g or more, 0.0030 cm 3 / g or more, 0.0030 cm 3 / g more than, 0.0032 cm 3 / g or more, 0.0034 cm 3 / g or more, 0.0035 cm 3 / g or more, 0.0036 cm 3 / g or more, or 0.0038 cm 3It may be greater than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 1.4 to 3.0 nm in the pore distribution curve is 0.0040 cm³. 3 / g or more, 0.0040cm 3 / g, 0.0042cm 3 / g or more, 0.0044cm 3 / g or more, 0.0045cm 3 / g or more, 0.0046cm 3 / g or more, 0.0048cm 3 / g or more, 0.0050cm 3 / g or more, 0.0050cm 3 / g, 0.0052cm 3 / g or more, 0.0054cm 3 / g or more, 0.0056cm 3 / g or more, 0.0058cm 3 / g or more, 0.0060cm 3 / g or more, 0.0060cm 3 / g, 0.0062cm 3 / g or more, or 0.0064 cm 3 It may be greater than or equal to / g. From these viewpoints, the cumulative value of the differential pore volume in the pore diameter range of 1.4 to 3.0 nm in the pore distribution curve should be 0.0010 to 0.0080 cm³. 3 / g, 0.0010–0.0065cm 3 / g, 0.0010-0.0055cm 3 / g, 0.0010-0.0045cm 3 / g, 0.0020–0.0080 cm 3 / g, 0.0020-0.0065cm 3 / g, 0.0020–0.0055cm 3 / g, 0.0025–0.0045 cm 3 / g, 0.0030–0.0080 cm 3 / g, 0.0030–0.0065cm 3 / g, 0.0030-0.0055cm 3 / g, 0.0030–0.0045cm 3 / g, 0.0040–0.0080 cm 3 / g, 0.0040–0.0065cm 3 / g, 0.0040-0.0055cm3 / g, or 0.0040 to 0.0045 cm 3 It can be / g.

[0039] The integrated value of the differential pore volume in the pore diameter range of 10–30 nm in the pore distribution curve of cerium oxide particles can be considered as the pore volume of pores with a diameter of 10–30 nm, and these pores are thought to represent pores between cerium oxide particles. The integrated value of the differential pore volume in the pore diameter range of 10–30 nm in the pore distribution curve tends to suppress the aggregation of cerium oxide particles, and the increased number of reaction sites on the surface of cerium oxide particles makes it easier to improve chemical reactivity and thus improve the polishing rate of insulating materials. From this perspective, 0.010 cm is considered appropriate. 3 / g or more, 0.012cm 3 / g or more, 0.014cm 3 / g or more, 0.016cm 3 / g or more, 0.018cm 3 / g or more, 0.020cm 3 / g or more, 0.020cm 3 / g, 0.022cm 3 / g or more, 0.024cm 3 / g or more, 0.026cm 3 / g or more, 0.028cm 3 / g or more, 0.030cm 3 / g or more, 0.030cm 3 / g, 0.032cm 3 / g or more, 0.034cm 3 / g or more, 0.035cm 3 / g or more, 0.036cm 3 / g or more, or 0.037 cm 3 It may be greater than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore distribution curve is 0.038 cm³. 3 / g or more, 0.040cm 3 / g or more, 0.040cm 3 / g, 0.042cm 3 / g or more, 0.044cm 3 / g or more, 0.046cm 3 / g or more, 0.048cm 3 / g or more, 0.050cm3 / g or more, 0.050cm 3 / g, 0.052cm 3 / g or more, 0.054cm 3 / g or more, 0.056cm 3 / g or more, 0.058cm 3 / g or more, 0.060cm 3 / g or more, 0.062cm 3 / g or more, or 0.064 cm 3 It may be greater than or equal to / g. The integrated value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore distribution curve should be 0.080 cm², from the viewpoint of easily increasing the physical strength of cerium oxide particles and easily improving the polishing speed of insulating materials. 3 / g or less, 0.075cm 3 / g or less, 0.070cm 3 Less than or equal to 0.065 cm² 3 It may be less than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore distribution curve is 0.060 cm³. 3 / g or less, 0.055cm 3 / g or less, 0.054cm 3 / g or less, 0.052cm 3 / g or less, 0.050cm 3 / g or less, 0.050cm 3 Less than 0.048 cm / g 3 / g or less, 0.046cm 3 / g or less, 0.045cm 3 / g or less, 0.044cm 3 / g or less, 0.043cm 3 / g or less, 0.042cm 3 / g or less, 0.040cm 3 / g or less, 0.040cm 3 Less than 0.038 cm / g 3 Less than or equal to 0.037 cm² 3 It may be less than or equal to / g. From these viewpoints, the cumulative value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore distribution curve should be 0.010 to 0.080 cm³. 3 / g, 0.010–0.070 cm 3 / g, 0.010–0.065cm 3 / g, 0.010–0.050cm 3 / g, 0.010–0.045cm 3 / g, 0.020–0.080 cm 3 / g, 0.020–0.070 cm 3 / g, 0.020–0.065cm 3 / g, 0.020-0.050cm 3 / g, 0.020–0.045cm 3 / g, 0.030–0.080 cm 3 / g, 0.030–0.070 cm 3 / g, 0.030–0.065cm 3 / g, 0.030-0.050cm 3 / g, 0.040–0.045cm 3 / g, 0.037–0.080 cm 3 / g, 0.037–0.070 cm 3 / g, 0.037–0.065cm 3 / g, 0.037–0.050 cm 3 / g, or 0.037–0.045 cm 3 It can be / g.

[0040] The integrated value of the differential pore volume in the pore diameter range of 10–180 nm in the pore distribution curve of cerium oxide particles can be considered as the pore volume of pores in the pore diameter range of 10–180 nm. The integrated value of the differential pore volume in the pore diameter range of 10–180 nm in the pore distribution curve tends to suppress aggregation of cerium oxide particles, leading to an increase in reaction sites on the surface of cerium oxide particles, which improves chemical reactivity and thus improves the polishing speed of insulating materials. Therefore, 0.12 cm is considered appropriate. 3 It may be greater than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 10 to 180 nm in the pore distribution curve is 0.13 cm³. 3 / g or more, 0.14cm 3 / g or more, 0.15cm 3 / g or more, or 0.16cm 3 It may be greater than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 10 to 30 nm in the pore distribution curve should be 0.16 cm, from the viewpoint of easily increasing the physical strength of cerium oxide particles and easily improving the polishing speed of the insulating material.3 It may be less than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 10 to 180 nm in the pore distribution curve is 0.15 cm³. 3 / g or less, 0.14cm 3 / g or less, 0.13cm 3 / g or less, or 0.12 cm 3 It may be less than or equal to / g. From these viewpoints, the cumulative value of the differential pore volume in the pore diameter range of 10 to 180 nm in the pore distribution curve should be 0.11 to 0.16 cm³. 3 / g, 0.11-0.15cm 3 / g, 0.12-0.17cm 3 / g, 0.12–0.16cm 3 / g, 0.12-0.15cm 3 / g, 0.13–0.17cm 3 / g, 0.13–0.16cm 3 / g, or 0.13-0.15cm 3 It can be / g.

[0041] The integrated value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve of cerium oxide particles can be considered as the total pore volume. The integrated value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve tends to suppress aggregation of cerium oxide particles, leading to an increase in reaction sites on the surface of cerium oxide particles, which improves chemical reactivity and thus improves the polishing speed of insulating materials. Therefore, 0.50 cm is considered appropriate. 3 / g or less, 0.40cm 3 / g or less, 0.35cm 3 / g or less, 0.30cm 3 / g or less, 0.28cm 3 / g or less, 0.26cm 3 / g or less, 0.25cm 3 / g or less, 0.24cm 3 / g or less, 0.22cm 3 / g or less, 0.21cm 3 / g or less, 0.20cm 3 / g or less, 0.19cm 3 Less than or equal to 0.18 cm / g 3It may be less than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve is 0.17 cm³. 3 / g or less, 0.16cm 3 / g or less, 0.15cm 3 / g or less, or 0.14 cm 3 It may be less than or equal to / g. The integrated value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve should be 0.05 cm, from the viewpoint of easily increasing the physical strength of cerium oxide particles and easily improving the polishing speed of the insulating material. 3 / g or more, 0.08cm 3 / g or more, 0.10cm 3 / g or more, 0.10cm 3 > / g, 0.11cm 3 / g or more, 0.12cm 3 / g or more, 0.13cm 3 / g or more, or 0.14cm 3 It may be greater than or equal to / g. The cumulative value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve is 0.15 cm³. 3 / g or more, 0.16cm 3 / g or more, 0.17cm 3 / g or more, or 0.18cm 3 It may be 1 / g or more. From these viewpoints, the cumulative value of the differential pore volume in the pore diameter range of 1.4 to 180 nm in the pore distribution curve should be 0.05 to 0.50 cm³. 3 / g, 0.05-0.30cm 3 / g, 0.05-0.21cm 3 / g, 0.05-0.20cm 3 / g, 0.05-0.19cm 3 / g, 0.10-0.50cm 3 / g, 0.10-0.30cm 3 / g, 0.10-0.21cm 3 / g, 0.10-0.20cm 3 / g, 0.10-0.19cm 3 / g, 0.12-0.50cm 3 / g, 0.12-0.30cm 3 / g, 0.12–0.21cm 3 / g, 0.12-0.20cm 3 / g, 0.12–0.19cm 3 / g, 0.14-0.50cm 3 / g, 0.14–0.30cm 3 / g, 0.14–0.21cm 3 / g, 0.14-0.20cm 3 / g, or 0.14-0.19 cm 3 It can be / g.

[0042] Methods for adjusting the BET specific surface area, BET diameter, crystallite diameter, and the integrated value of the differential pore volume within a specific pore diameter range in the pore distribution curve include changing the composition of the raw materials; changing the method of preparing the raw materials; changing the firing temperature, firing time, heating rate, cooling rate, and atmospheric gas in the firing method; and changing the grinding method and conditions. These methods may be used individually or in combination. For example, lowering the firing temperature in the firing method tends to increase the BET specific surface area, decrease the BET diameter, and decrease the crystallite diameter.

[0043] The cerium oxide particles to be measured for obtaining the BET specific surface area, crystallite size, etc., may be recovered by drying the slurry (to dryness), or by separating and removing components other than cerium oxide particles from the dried material. If the BET specific surface area, crystallite size, etc., of the cerium oxide particles do not change during slurry preparation, the cerium oxide particles to be measured may be the cerium oxide particles before mixing with other components such as water.

[0044] The average particle size of the abrasive grains, or the average particle size of the cerium oxide particles, may be within the following ranges. The average particle size may be 100 nm or more, 150 nm or more, 175 nm or more, greater than 175 nm, 180 nm or more, 200 nm or more, or 205 nm or more, from the viewpoint of easily obtaining a high polishing speed for insulating materials. The average particle size may be 210 nm or more, 215 nm or more, 220 nm or more, 225 nm or more, 230 nm or more, or 235 nm or more. The average particle size may be 600 nm or less, 550 nm or less, less than 550 nm, 500 nm or less, 450 nm or less, 400 nm or less, 350 nm or less, 320 nm or less, 300 nm or less, 295 nm or less, 290 nm or less, 285 nm or less, 280 nm or less, 275 nm or less, 270 nm or less, 265 nm or less, 260 nm or less, 255 nm or less, 250 nm or less, 245 nm or less, or 240 nm or less, from the viewpoint of easily reducing scratches caused by polishing. From these perspectives, the average particle size may be 100-600 nm, 100-500 nm, 100-400 nm, 100-300 nm, 100-280 nm, 100-250 nm, 150-600 nm, 150-500 nm, 150-400 nm, 150-300 nm, 150-280 nm, 150-250 nm, 200-600 nm, 200-500 nm, 200-400 nm, 200-300 nm, 200-280 nm, 200-250 nm, 250-600 nm, 250-500 nm, 250-400 nm, 250-300 nm, or 250-280 nm.

[0045] The average particle size is the average particle size based on volume, and refers to the MV (volume average diameter) value measured with a laser diffraction particle size analyzer. For example, it can be measured by the method described in the examples below. The average particle size (volume average diameter) may be measured by diluting the slurry with water to adjust the abrasive content or cerium oxide particle content to an appropriate level. For example, in the case of the product name "SYNC" manufactured by Microtrac-Bell Corporation, the content may be adjusted to a DV (Diffraction Volume) value of 0.0010 to 0.0150. The DV value is a concentration index that utilizes the total amount of scattered light from the sample received by the detector, and tends to increase as the abrasive content or cerium oxide particle content in the sample increases. If a slurry containing abrasive grains (abrasive grains containing cerium oxide particles), additives, and water is stored separately as a first liquid containing abrasive grains and water, and a second liquid containing additives and water, the abrasive grain content may be adjusted to an appropriate level by diluting the first liquid with water, and the average particle size may be measured.

[0046] Methods for adjusting the average particle size include adjusting the composition of the raw materials, the manufacturing method, the firing temperature, the firing time, etc.; grinding; classification; and filtration. Grinding, classification, and filtration may be performed on abrasive grains or cerium oxide particles, or on raw materials for obtaining cerium oxide particles (cerium compounds such as cerium carbonate).

[0047] The abrasive content in the slurry, or the cerium oxide particle content in the slurry, may be within the following ranges based on the total mass of the slurry. The content may be 0.01% by mass or more, 0.05% by mass or more, 0.10% by mass or more, 0.15% by mass or more, 0.30% by mass or more, 0.50% by mass or more, 0.80% by mass or more, 1.00% by mass or more, 1.20% by mass or more, 1.50% by mass or more, 1.80% by mass or more, or 2.00% by mass or more, from the viewpoint of easily obtaining a high polishing speed for insulating materials. The content may be 20.00% by mass or less, 15.00% by mass or less, 10.00% by mass or less, 8.00% by mass or less, 5.00% by mass or less, 4.50% by mass or less, 4.00% by mass or less, 3.50% by mass or less, 3.00% by mass or less, 2.50% by mass or less, or 2.00% by mass or less, from the viewpoint of suppressing particle aggregation and making it less likely to scratch the polished surface. From these perspectives, the content may be 0.01 to 20.00 mass%, 0.01 to 10.00 mass%, 0.01 to 5.00 mass%, 0.10 to 20.00 mass%, 0.10 to 10.00 mass%, 0.10 to 5.00 mass%, 0.50 to 20.00 mass%, 0.50 to 10.00 mass%, 0.50 to 5.00 mass%, 1.00 to 20.00 mass%, 1.00 to 10.00 mass%, or 1.00 to 5.00 mass%.

[0048] (Water) There are no particular restrictions on the type of water used, but examples include deionized water and ultrapure water. The water content is not particularly limited and may be the remainder of the slurry after removing the content of other components.

[0049] The water content in the slurry may be within the following ranges, based on the total mass of the slurry, from the viewpoint of obtaining a high polishing speed for the insulating material while suppressing a decrease in polishing speed as polishing progresses. The water content may be 50% by mass or more, 70% by mass or more, 80% by mass or more, 90% by mass or more, 93% by mass or more, 95% by mass or more, 96% by mass or more, or 97% by mass or more. The water content may be less than 100% by mass, 99% by mass or less, or 98% by mass or less. From these viewpoints, the water content may be 50% by mass or more and less than 100% by mass, 50 to 99% by mass, 50 to 98% by mass, 80% by mass or more and less than 100% by mass, 80 to 99% by mass, 80 to 98% by mass, 90% by mass or more and less than 100% by mass, 90 to 99% by mass, or 90 to 98% by mass.

[0050] (Additives) The slurry according to this embodiment may or may not contain any additives. Examples of optional additives include polar solvents (ethanol, acetone, etc.), materials having carboxyl groups (excluding compounds corresponding to polyoxyalkylene compounds or water-soluble polymers), polyoxyalkylene compounds, water-soluble polymers, oxidizing agents (e.g., hydrogen peroxide), and dispersants (e.g., phosphate-based inorganic salts).

[0051] Materials containing a carboxyl group include monocarboxylic acids such as acetic acid, propionic acid, butyric acid, and valeric acid; hydroxy acids such as lactic acid, malic acid, and citric acid; dicarboxylic acids such as malonic acid, succinic acid, fumaric acid, and maleic acid; and amino acids such as arginine, histidine, and lysine.

[0052] Examples of polyoxyalkylene compounds include polyalkylene glycols and polyoxyalkylene derivatives.

[0053] Examples of polyalkylene glycols include polyethylene glycol, polypropylene glycol, and polybutylene glycol.

[0054] Polyoxyalkylene derivatives are, for example, compounds obtained by introducing a functional group or substituent to a polyalkylene glycol, or compounds obtained by adding a polyalkylene oxide to an organic compound. Examples of functional groups or substituents include alkyl ether groups, alkylphenyl ether groups, phenyl ether groups, styrene-phenyl ether groups, glyceryl ether groups, alkylamine groups, fatty acid ester groups, glycol ester groups, and the like. Examples of polyoxyalkylene derivatives include polyoxyethylene alkyl ethers, polyoxyethylene bisphenol ethers (e.g., BA Glycol series from Nippon Emulsifier Co., Ltd.), polyoxyethylene styrene-phenyl ethers (e.g., Emulgen series from Kao Corporation), polyoxyethylene alkylphenyl ethers (e.g., Neugen EA series from Daiichi Kogyo Seiyaku Co., Ltd.), polyoxyalkylene polyglyceryl ethers (e.g., SC-E series and SC-P series from Sakamoto Pharmaceutical Co., Ltd.), polyoxyethylene sorbitan fatty acid esters (e.g., Sorgen TW series from Daiichi Kogyo Seiyaku Co., Ltd.), polyoxyethylene fatty acid esters (e.g., Emanon series from Kao Corporation), polyoxyethylene alkylamines (e.g., Amiradin D from Daiichi Kogyo Seiyaku Co., Ltd.), and other compounds to which polyalkylene oxides have been added (e.g., Surfinol 465 from Nisshin Chemical Industry Co., Ltd.; TMP series from Nippon Emulsifier Co., Ltd.).

[0055] Water-soluble polymers have the effect of adjusting the dispersion stability of abrasive particles. A "water-soluble polymer" is defined as a polymer that dissolves at a rate of 0.1 g or more per 100 g of water. Polymers that fall under the category of polyoxyalkylene compounds are not included in the definition of a "water-soluble polymer."

[0056] Examples of water-soluble polymers include polycarboxylic acids such as polyacrylic acid and polymaleic acid; acrylic polymers such as polyacrylamide and polydimethylacrylamide; polysaccharides such as carboxymethylcellulose, agar, curdlan, dextrin, cyclodextrin, and pullulan; vinyl polymers such as polyvinyl alcohol, polyvinylpyrrolidone, and polyacrolein; and glycerin polymers such as polyglycerin and polyglycerin derivatives.

[0057] The content of the water-soluble polymer may be within the following ranges based on the total mass of the slurry, from the viewpoint of easily obtaining the effect of adding the water-soluble polymer while suppressing the settling of abrasive grains. The content of the water-soluble polymer may be 0.001% by mass or more, 0.005% by mass or more, 0.010% by mass or more, 0.020% by mass or more, 0.030% by mass or more, 0.040% by mass or more, 0.050% by mass or more, 0.060% by mass or more, 0.070% by mass or more, or 0.075% by mass or more. The content of the water-soluble polymer may be 10.000 mass% or less, 8.000 mass% or less, 6.000 mass% or less, 5.000 mass% or less, 3.000 mass% or less, 1.000 mass% or less, 0.500 mass% or less, 0.300 mass% or less, 0.100 mass% or less, 0.080 mass% or less, or 0.075 mass% or less. From these perspectives, the content of the soluble polymer may be 0.001 to 10.000% by mass, 0.001 to 1.000% by mass, 0.001 to 0.500% by mass, 0.001 to 0.100% by mass, 0.010 to 10.000% by mass, 0.010 to 1.000% by mass, 0.010 to 0.500% by mass, 0.010 to 0.100% by mass, 0.030 to 10.000% by mass, 0.030 to 1.000% by mass, 0.030 to 0.500% by mass, 0.030 to 0.100% by mass, 0.050 to 10.000% by mass, 0.050 to 1.000% by mass, 0.050 to 0.500% by mass, or 0.050 to 0.100% by mass.

[0058] (pH) The pH of the slurry according to this embodiment may be within the following ranges. From the viewpoint of easily obtaining a high polishing speed for the insulating material, the pH may be 1.0 or higher, 1.5 or higher, 2.0 or higher, 2.5 or higher, 3.0 or higher, greater than 3.0, 3.5 or higher, greater than 3.5, 4.0 or higher, greater than 4.0, 4.1 or higher, 4.2 or higher, 4.3 or higher, 4.4 or higher, 4.5 or higher, greater than 4.5, 4.6 or higher, 4.7 or higher, 4.8 or higher, 4.9 or higher, 5.0 or higher, greater than 5.0, 5.1 or higher, or 5.2 or higher. The pH may be 5.3 or higher, 5.4 or higher, 5.5 or higher, greater than 5.5, 5.6 or higher, 5.7 or higher, 5.8 or higher, or 5.9 or higher. From the viewpoint of improving the storage stability of the slurry, the pH may be 7.0 or less, less than 7.0, 6.5 or less, less than 6.5, 6.4 or less, 6.2 or less, 6.0 or less, less than 6.0, or 5.9 or less. The pH may be 5.8 or less, 5.7 or less, 5.6 or less, 5.5 or less, 5.4 or less, or 5.3 or less. From these viewpoints, the pH may be 1.0 to 7.0, 1.0 to 6.0, 2.0 to 7.0, 2.0 to 6.0, 3.0 to 7.0, 3.0 to 6.0, 4.0 to 7.0, 4.0 to 6.0, 4.5 to 7.0, 4.5 to 6.0, 5.0 to 7.0, or 5.0 to 6.0. The pH of the slurry is defined as the pH at a liquid temperature of 25°C.

[0059] The pH of the slurry can be adjusted by acidic components such as inorganic acids and organic acids; and alkaline components such as ammonia, sodium hydroxide, tetramethylammonium hydroxide (TMAH), imidazole, and alkanolamines. A buffering agent may be added to stabilize the pH, or a buffer solution (a solution containing a buffering agent) may be added. Examples of buffer solutions include acetate buffers and phthalate buffers.

[0060] The pH of the slurry according to this embodiment can be measured using a pH meter (for example, model PHL-40 manufactured by Toa DKK Corporation). For example, after calibrating the pH meter at two points using phthalate pH buffer (pH: 4.01) and neutral phosphate pH buffer (pH: 6.86) as standard buffers, the pH meter electrode can be placed in the slurry, and the value after stabilization for two minutes or more can be measured as the pH of the slurry. The liquid temperature of both the standard buffer and the slurry should be 25°C.

[0061] (Storage Method) When the slurry according to this embodiment contains any of the above-mentioned additives, the slurry according to this embodiment may be stored in a single-liquid state containing abrasive grains, additives, and water, or it may be stored as a multi-liquid slurry (slurry set) in which the components of the slurry are divided into a first liquid and a second liquid so that the slurry is formed by mixing a first liquid containing abrasive grains and water with a second liquid containing additives and water. The slurry according to this embodiment may be in a single-liquid state containing abrasive grains, additives, and water, or it may be the first liquid in a multi-liquid slurry. The second liquid may contain at least one of the additives, and the first liquid may contain the same or different additive as the additive in the second liquid. The components of the slurry may be stored in three or more liquids.

[0062] In the multi-liquid slurry described above, the first liquid and the second liquid are mixed immediately before or during polishing to prepare the slurry. The single-liquid slurry can be stored as a storage liquid with reduced water content and may be diluted with water before use during polishing. In the multi-liquid slurry, the first liquid and the second liquid can be stored as a storage liquid with reduced water content and may be diluted with water before use during polishing.

[0063] <Polishing Method> The polishing method according to this embodiment (polishing method for a substrate, etc.) comprises a polishing step of polishing the surface to be polished (the surface to be polished of a substrate, etc.) using the slurry according to this embodiment. The slurry in the polishing step may be a slurry obtained by mixing the first liquid and the second liquid in the multi-liquid slurry described above.

[0064] In the polishing process, for example, the insulating material of a substrate having an insulating material may be pressed against the polishing pad (polishing cloth) of a polishing platen, and the slurry according to this embodiment may be supplied between the material to be polished and the polishing pad, and the substrate and the polishing platen may be moved relative to each other to polish the surface of the insulating material. In the polishing process, for example, at least a portion of the insulating material is removed by polishing.

[0065] Examples of substrates to be polished include substrates to be polished. Examples of substrates to be polished include substrates used in semiconductor device manufacturing (e.g., semiconductor substrates on which STI patterns, gate patterns, wiring patterns, etc., are formed) on which an insulating material is formed. Examples of insulating materials include silicon oxide. The insulating material may be a single material or multiple materials. If multiple materials are exposed on the surface to be polished, they can be considered as insulating materials. The insulating material may be in the form of a film (insulating film) or a silicon oxide film.

[0066] By using the slurry according to this embodiment, the surface irregularities of the insulating material (e.g., silicon oxide) formed on the substrate can be polished to remove excess material, thereby eliminating surface irregularities and obtaining a smooth surface across the entire surface of the insulating material.

[0067] In the polishing method according to this embodiment, a general polishing apparatus can be used, which includes a holder capable of holding a substrate having a surface to be polished, and a polishing platen to which a polishing pad can be attached. A motor with a changeable rotation speed may be attached to each of the holder and the polishing platen.

[0068] As polishing pads, general nonwoven fabrics, foams, and non-foamed materials can be used. As materials for polishing pads, resins such as polyurethane, acrylic resin, polyester, acrylic-ester copolymer, polytetrafluoroethylene, polypropylene, polyethylene, poly-methylpentene, cellulose, cellulose ester, polyamide (e.g., nylon (trademark name) and aramid), polyimide, polyimidamide, polysiloxane copolymer, oxirane compounds, phenolic resin, polystyrene, polycarbonate, and epoxy resin can be used. From the viewpoint of easily obtaining excellent polishing speed and flatness, the material of the polishing pad may be at least one selected from the group consisting of foamed polyurethane and non-foamed polyurethane. The polishing pad may be grooved to allow slurry to accumulate.

[0069] There are no restrictions on the polishing conditions, but the upper limit of the polishing platen's rotation speed is 200 mins to prevent the base material from flying off. -1 (min-1 The pressure (rpm) may be less than or equal to 100 kPa, and the upper limit of the polishing pressure (processing load) applied to the substrate may be 100 kPa or less, from the viewpoint of easily suppressing the occurrence of polishing scratches. During polishing, slurry may be continuously supplied to the polishing pad by a pump or the like. There is no limit to the amount of slurry supplied in this case, but the surface of the polishing pad may always be covered with slurry.

[0070] The slurry and polishing method according to this embodiment may be used to polish a surface containing silicon oxide, and may be used to polish a surface containing silicon oxide derived from TEOS (tetraethoxysilane) (silicon oxide obtained using TEOS). The slurry and polishing method according to this embodiment can be suitably used for the formation of STI and high-speed polishing of interlayer insulating materials. Such silicon oxide may have some of its constituent elements substituted with carbon atoms, nitrogen atoms, etc.

[0071] The slurry and polishing method according to this embodiment can also be used for polishing premetallic insulating materials. Examples of premetallic insulating materials include silicon oxide, phosphorus-silicate glass, boron-phosphorus-silicate glass, silicon oxyfluoride, amorphous carbon fluoride, and the like.

[0072] The slurry and polishing method according to this embodiment can be applied to materials other than insulating materials such as silicon oxide. Examples of such materials include high dielectric constant materials such as Hf-based, Ti-based, and Ta-based oxides; semiconductor materials such as silicon, amorphous silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, and organic semiconductors; phase change materials such as GeSbTe; inorganic conductive materials such as ITO; and polymer resin materials such as polyimide-based, polybenzoxazole-based, acrylic-based, epoxy-based, and phenol-based materials.

[0073] The slurry and polishing method according to this embodiment can be applied not only to film-like polishing targets, but also to various substrates made of glass, silicon, SiC, SiGe, Ge, GaN, GaP, GaAs, sapphire, plastic, and the like.

[0074] The slurry and polishing method according to this embodiment can be used not only for the manufacture of semiconductor devices, but also for the manufacture of image display devices such as TFTs and organic ELs; optical components such as photomasks, lenses, prisms, optical fibers, and single-crystal scintillators; optical elements such as optical switching elements and optical waveguides; light-emitting elements such as solid-state lasers and blue laser LEDs; and magnetic storage devices such as magnetic disks and magnetic heads.

[0075] <Manufacturing Method, etc.> The manufacturing method of a component according to this embodiment includes a component manufacturing step of obtaining a component using a workpiece (substrate) polished by the polishing method according to this embodiment. The component according to this embodiment is a component obtained by the manufacturing method of a component according to this embodiment. The component according to this embodiment is not particularly limited, but may be an electronic component (for example, a semiconductor component such as a semiconductor package), a wafer (for example, a semiconductor wafer), or a chip (for example, a semiconductor chip). As one embodiment of the manufacturing method of a component according to this embodiment, the manufacturing method of an electronic component according to this embodiment obtains an electronic component using a workpiece polished by the polishing method according to this embodiment. As one embodiment of the manufacturing method of a component according to this embodiment, the manufacturing method of a semiconductor component according to this embodiment obtains a semiconductor component (for example, a semiconductor package) using a workpiece polished by the polishing method according to this embodiment. The manufacturing method of a component according to this embodiment may include a polishing step of polishing the workpiece using the polishing method according to this embodiment before the component manufacturing step.

[0076] As one aspect of the component manufacturing process according to this embodiment, the component manufacturing process may include a piece-forming step in which the member to be polished (substrate) polished by the polishing method according to this embodiment is divided into individual pieces. The piece-forming step may be, for example, a step of dicing a wafer (e.g., a semiconductor wafer) polished by the polishing method according to this embodiment to obtain a chip (e.g., a semiconductor chip). As one aspect of the component manufacturing process according to this embodiment, the electronic component manufacturing process according to this embodiment may include a step of obtaining an electronic component (e.g., a semiconductor component) by dividing the member to be polished by the polishing method according to this embodiment into individual pieces. As one aspect of the component manufacturing process according to this embodiment, the semiconductor component manufacturing process according to this embodiment may include a step of obtaining a semiconductor component (e.g., a semiconductor package) by dividing the member to be polished by the polishing method according to this embodiment into individual pieces.

[0077] The method for manufacturing a part according to this embodiment may include, as one aspect of the part manufacturing process, a connection step of connecting (for example, electrically connecting) a member to be polished (substrate) polished by the polishing method according to this embodiment to another connected body. The connected body connected to the member to be polished by the polishing method according to this embodiment is not particularly limited and may be the member to be polished by the polishing method according to this embodiment, or it may be a connected body different from the member to be polished by the polishing method according to this embodiment. In the connection step, the member to be polished and the connected body may be directly connected (connected in a state where the member to be polished and the connected body are in contact), or they may be connected via another member (such as a conductive member). The connection step can be performed before the individualization step, after the individualization step, or before and after the individualization step.

[0078] The connection step may be a step of connecting the surface of the member to be polished, which has been polished by the polishing method according to this embodiment, to the connected body, or a step of connecting the connecting surface of the member to be polished, which has been polished by the polishing method according to this embodiment, to the connecting surface of the connected body. The connecting surface of the member to be polished may be the surface of the member to be polished, which has been polished by the polishing method according to this embodiment. By the connection step, a connected body comprising the member to be polished and the connected body can be obtained. In the connection step, if the connecting surface of the member to be polished has a metal part, the connected body may be brought into contact with the metal part. In the connection step, if the connecting surface of the member to be polished has a metal part and the connecting surface of the connected body has a metal part, the metal parts may be brought into contact with each other. The metal part may contain copper.

[0079] The device according to this embodiment (for example, an electronic device such as a semiconductor device) comprises a member to be polished by the polishing method according to this embodiment, and at least one selected from the group consisting of the component according to this embodiment.

[0080] <Cerium Oxide Particles> The cerium oxide particles according to this embodiment have a ratio of BET diameter to crystallite diameter of 1.00 or more in the (111) plane, and the integrated value of the differential pore volume in the range of pore diameters from 10 to 180 nm in the pore distribution curve is 0.11 to 0.17 cm². 3 The weight is / g. The cerium oxide particles according to this embodiment can be used as abrasive grains in the slurry described above. The cerium oxide particles can be obtained by the method described above. The cerium oxide particles have a BET diameter ratio of 1.00 or more to the crystallite diameter, and the integrated value of the differential pore volume in the range of pore diameters from 10 to 180 nm in the pore distribution curve is 0.11 to 0.17 cm². 3 As long as the value is / g, the cerium oxide particles may be before or after at least one treatment selected from the group consisting of grinding and classification. The BET specific surface area, BET diameter, crystallite diameter on the (111) plane, ratio of BET diameter to crystallite diameter on the (111) plane, and integrated value of differential pore volume for a specific range of pore diameters in the pore distribution curve may be within or outside the above range.

[0081] The average particle size of the cerium oxide particles may be 0.1 μm or more, 0.5 μm or more, 1 μm or more, or 5 μm or more, and may be 50 μm or less, 40 μm or less, 30 μm or less, 20 μm or less, or 10 μm or less. The average particle size of the cerium oxide particles may be 0.1 to 50 μm, 0.1 to 30 μm, or 0.1 to 10 μm. The average particle size of the cerium oxide particles may be within the range of the average particle size of the cerium oxide particles in the slurry described above. The average particle size of the cerium oxide particles can be measured by the same method as for the cerium oxide particles in the slurry described above.

[0082] The present disclosure will be described in detail below based on examples, but the present disclosure is not limited to the following examples.

[0083] <Preparation of Slurry> Cerium oxide particles were prepared, and a polishing slurry was obtained by mixing the cerium oxide particles (abrasive grains), pure water, and polyglycerin (manufactured by Sakamoto Pharmaceutical Co., Ltd., product name: Polyglycerin #750) in a mass ratio of 2.000:97.925:0.075. The physical properties of the cerium oxide particles in the slurries prepared in each example and comparative example are shown in Table 1.

[0084] (Example 1) (Preparation of Cerium Oxide Particles) Based on the "extraction method" described above, a cerium carbonate precipitate was produced by mixing a 0.1 mol / L aqueous solution of cerium(III) sulfate and a 0.1 mol / L aqueous solution of sodium carbonate in a volume ratio of 1:2 while maintaining each at 95°C. This precipitate was filtered and dried to obtain cerium carbonate powder (raw material). The cerium carbonate powder was placed in an alumina container and heated in air using an AS ONE HPM-2N oven at a rate of 0.6°C / min to 400°C, then heated to 550°C at a rate of 13.3°C / min for 1 hour. After that, it was cooled by air cooling (air flow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 120 minutes) to obtain a white powder. Phase identification of this powder was performed by XRD and confirmed to be cerium oxide. The obtained cerium oxide powder was crushed in a mortar and then passed through a sieve with a mesh size of 450 μm. The resulting powder, pure water, and acetic acid were mixed in a mass ratio of 20.00:79.94:0.06 and ground using a bead mill for 10 minutes. The resulting dispersion was centrifuged for 60 seconds using a Hitachi Koki himac CR7 centrifuge (rotation speed 2000 rpm), and the liquid remaining at the top of the container after centrifugation was obtained as a dispersion containing cerium oxide particles.

[0085] (Preparation of slurry) Cerium oxide particles were prepared, and a polishing slurry was obtained by mixing the cerium oxide particles (abrasive grains), pure water, and polyglycerin (manufactured by Sakamoto Pharmaceutical Co., Ltd., product name: Polyglycerin #750) in a mass ratio of 2.000:97.925:0.075. The physical properties of the cerium oxide particles in the slurry prepared in each example and comparative example are shown in Table 1.

[0086] (Example 2) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.5°C / min.

[0087] (Example 3) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.4°C / min.

[0088] (Example 4) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.5°C / min and the mixture was cooled by air cooling (atmospheric flow) at an average cooling rate of 5.00°C / min (cooled to 100°C in 90 minutes).

[0089] (Example 5) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the firing temperature was set to 450°C and the mixture was cooled by air cooling (airflow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 93.3 minutes).

[0090] (Example 6) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.5°C / min, the firing temperature was 450°C, and the mixture was cooled by air cooling (airflow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 93.3 minutes).

[0091] (Example 7) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.4°C / min, the firing temperature was 450°C, and the mixture was cooled by air cooling (airflow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 93.3 minutes).

[0092] (Example 8) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.5°C / min, the firing temperature was 430°C, and the mixture was cooled by air cooling (atmospheric flow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 88 minutes).

[0093] (Example 9) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate to 400°C was 0.4°C / min, the firing temperature was 430°C, and the mixture was cooled by air cooling (atmospheric flow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 88 minutes).

[0094] (Comparative Example 1) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that it was cooled by air cooling (natural cooling) at an average cooling rate of 1.88°C / min (cooled to 100°C in 240 minutes).

[0095] (Comparative Example 2) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate was set to 13.3°C / min over the entire range.

[0096] (Comparative Example 3) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the heating rate was set to 13.3°C / min over the entire range, the firing temperature was set to 430°C, and the mixture was cooled by air cooling (atmospheric flow) at an average cooling rate of 3.75°C / min (cooled to 100°C in 88 minutes).

[0097] (Comparative Example 4) A dispersion containing cerium oxide particles was obtained in the same manner as in Example 1, except that the firing temperature (natural cooling) was set to 750°C and the mixture was cooled by air cooling at an average cooling rate of 1.88°C / min (cooled to 100°C in 346 minutes).

[0098] <BET specific surface area, BET diameter, pore distribution curve> 75 g of each slurry described above was weighed into a commercially available evaporating dish and dried at 110°C for 15 hours. Next, vacuum drying was performed at room temperature (25°C) for 24 hours, followed by further vacuum drying at 100°C for 1 hour to obtain a dry product (cerium oxide particles). Next, 0.3 to 0.4 g of the dry product was weighed, and the BET specific surface area was measured using a BET specific surface area analyzer (Quantachrome Instruments, product name: QuadraSorb EVO) with liquid nitrogen (77 K) as the adsorption medium by gas adsorption method at a temperature of 77 K until the relative pressure reached 0.99, obtaining an adsorption isotherm when nitrogen was used as the adsorption medium. From the obtained adsorption isotherm, the BET specific surface area (S) of the cerium oxide particles was calculated by multipoint BET method in the relative pressure range of 0.049 to 0.30. N ) was obtained. Also, the obtained S N The BET diameter was calculated from the true density of the cerium oxide particles. Furthermore, a pore distribution curve was obtained from the adsorption isotherm when nitrogen was used as the adsorption medium, using QuadraWin (version 7.1) attached to the BET specific surface area measuring device, with the horizontal axis representing pore diameter and the vertical axis representing differential pore volume. From the obtained pore distribution curve, the integrated value of the differential pore volume in the range of pore diameter 1.4 nm to less than 3 nm, the integrated value of the differential pore volume in the range of pore diameter 10 to 30 nm, and the integrated value of the differential pore volume in the range of pore diameter 1.4 to 180 nm were calculated.

[0099] <True Density> 75 g of each slurry described above was weighed into a commercially available evaporating dish and dried at 110°C for 15 hours. Next, it was vacuum dried at room temperature (25°C) for 24 hours to obtain a dry product (cerium oxide particles). Then, 1 g of the dry product was weighed, and the true density was calculated using a true density analyzer (Microtrac-Bel, BELPYCNO) at a temperature of 25°C using the helium gas displacement method, based on the amount of helium gas filled and the weight of the sample.

[0100] <Cryslite Size> After placing each of the above slurries into a commercially available evaporating dish, the dry material (cerium oxide particles) was obtained by drying it in a dryer (Masuda Rika Kogyo Co., Ltd., SA-45, 110°C) for 24 hours. After crushing this dry material in a mortar, an X-ray diffraction pattern was obtained by performing an XRD measurement under the following conditions. Using Rigaku Corporation's "MiniFlex," the crystallite size of the cerium oxide particles at the (111) plane was calculated based on Scherrer's formula. During the analysis, measurement data of LaB6 was used as an external standard sample for linewidth (removal of linewidth originating from the instrument).

[0101] [XRD Measurement Conditions] XRD device: Sample horizontal type multi-purpose X-ray diffractometer Ultima IV (manufactured by Rigaku Corporation) X-ray source: CuKα rays Scanning method: 2θ / θ X-ray tube voltage: 40kV X-ray tube current: 15mA Receiving slit: OPEN Scan range: 10-120 deg Step: 0.02 deg Scanning speed: 4 deg / min

[0102] <Average particle size> Appropriate amounts of each of the above-mentioned slurries were placed into a laser diffraction particle size distribution analyzer (Microtrac-Bell Co., Ltd., product name "MT3300EXII", particle refractive index: 2.20), and the MV (volume average diameter) was obtained as the average particle size of the abrasive grains.

[0103] <pH of the slurry> The pH of each slurry described above (at 25°C) was measured using a pH meter, LAQUA twin (manufactured by Horiba, Ltd.).

[0104] <CMP Evaluation> Using the slurries described above, a CMP evaluation was conducted under the following conditions.

[0105] [CMP Polishing Conditions] Polishing equipment: Reflexion LK CMP (Applied Materials) Slurry flow rate: 250 mL / min Substrate to be polished: A blanket wafer without a pattern was used, and the substrate to be polished had a 2 μm thick silicon oxide film (silicon oxide film obtained using TEOS) on a silicon substrate. Polishing pad: Foamed polyurethane resin with closed cells (Nitta DuPont, model IK4250H) Polishing pressure: 27.6 kPa (4 psi) Rotation speed of substrate to be polished and polishing platen: Substrate to be polished / polishing platen = 117 / 123 rpm Polishing time: 20 seconds Wafer cleaning: After CMP treatment, the wafer was washed with water while applying ultrasound, and then dried with a spin dryer.

[0106] The polishing speed for a 20-second polishing period was determined for the silicon oxide film polished and cleaned under the conditions described above, using the following formula. The results are shown in Table 1. The difference in silicon oxide film thickness before and after polishing was determined using an optical interference film thickness analyzer (NOVA Corporation, product name: Nova i500). Polishing speed = Difference in silicon oxide film thickness before and after polishing [nm] / Polishing time [min]

[0107]

[0108]

Claims

It contains abrasive particles and water. The abrasive grains include cerium oxide particles, The ratio of the BET diameter to the crystallite diameter in the (111) plane of the cerium oxide particle is 1.00 or more. The cumulative value of the differential pore volume in the pore diameter range of 10 to 180 nm in the pore distribution curve of the cerium oxide particles is 0.11 to 0.17 cm³. 3 It is / g, slender.   The slurry according to claim 1, wherein the BET diameter is 21.0 nm or more.   The slurry according to claim 1, wherein the crystallite size is 23.0 nm or less.   The slurry according to claim 1, wherein the ratio is 1.70 or more.   The cumulative value of the differential pore volume in the range of pore diameters from 1.4 to 180 nm in the aforementioned pore distribution curve is 0.12 to 0.21 cm³. 3 The slurry according to claim 1, wherein the amount is / g.   The cumulative value of the differential pore volume in the pore diameter range of 1.4 to 3.0 nm in the aforementioned pore distribution curve is 0.0030 to 0.0065 cm³. 3 The slurry according to claim 1, wherein the amount is / g.   The slurry according to claim 1, wherein the abrasive content is 0.01 to 10.00% by mass.   The slurry according to claim 1, wherein the average particle size of the abrasive grains is 100 to 600 nm.   The slurry according to claim 1, wherein the pH is 1.0 to 7.

0. A polishing method comprising the step of polishing a member to be polished using a slurry according to any one of claims 1 to 8.   The polishing method according to claim 10, wherein the member to be polished contains silicon oxide.   A method for manufacturing a part, comprising the step of obtaining a part using the member to be polished by the polishing method described in claim 10. The ratio of the BET diameter to the crystallite diameter on the (111) plane is 1.00 or greater. The cumulative value of the differential pore volume in the pore diameter range of 10–180 nm in the pore distribution curve is 0.11–0.17 cm³. 3 Cerium oxide particles, weighing / g.