JP2020021824A - Polishing fine particle and method of producing the same - Google Patents

Abstract

To provide a polishing fine particle capable of polishing or grinding a hard-to-work substrate, such as an SiC substrate, a GaN substrate, a sapphire substrate, and a diamond substrate, at high rate (high polishing speed or high grinding speed) and also capable of stably maintaining high polishing quality, and a method of producing the same.SOLUTION: The present invention relates to a polishing fine particle and a method of producing the same. The polishing fine particle includes a diamond particle and a carbon-containing structure derived from a fullerene derivative, the structure being immobilized on a surface of the diamond particle. In a Raman spectrum obtained by light with an excitation wavelength of 532 nm, when ID represents the maximum intensity of a peak present in a region of 1,300-1,350 cm, I represents the maximum intensity of a peak present in a region of 1,400-1,500 cm, and IG represents the maximum intensity of a peak present in a region of 1,500-1,650 cm, the peaks being derived from the diamond particle, I/D is 0 or more and less than 0.05, and IG/ID is 0 or more and less than 0.005.SELECTED DRAWING: None

Description

  The present invention relates to polishing fine particles used for polishing (for example, chemical mechanical polishing: CMP) or grinding of difficult-to-process substrates such as a SiC substrate, a GaN substrate, a sapphire substrate, and a diamond substrate, and a method for producing the same.

  For the purpose of improving the polishing rate (polishing speed) and polishing quality in the chemical mechanical polishing (CMP) of SiC substrates used for power semiconductors, GaN substrates and diamond substrates, or sapphire substrates used for LED devices and the like. Various abrasive fine particles have been proposed.

  As such abrasive fine particles, for example, an abrasive in which fullerene or a fullerene compound is dispersed in a solvent (for example, Patent Document 1), an abrasive in which fullerene particles and silica particles are mixed in an alkaline solution (for example, Patent Document 2) Composite abrasive grains having base particles having a hydrophilic fullerene derivative adsorptivity on the surface and fullerene derivative coating layers formed by chemically bonding the fullerene derivatives adsorbed on the surface of the base particles (for example, see Patent Reference 3) has been proposed.

JP 2005-223278 A JP 2012-248594 A JP-A-2006-098354

  The polishing agent disclosed in Patent Document 1 has a problem in that, when used, the fullerene aggregates collapse due to external force applied during polishing and the particle size decreases, so that the polishing rate (polishing rate) gradually decreases. Further, in the polishing agent of Patent Document 2, when used, fullerene particles that modify the surface of the silica particles are dropped by external force applied during polishing, and the silica particles come into direct contact with the material to be polished, There is a problem that the surface roughness is increased and the possibility of occurrence of polishing scratches is increased. When a difficult-to-machine substrate is polished using the composite abrasive grains of Patent Document 3, the polishing rate (polishing rate) is not sufficient, and there is a problem that it may be difficult to complete polishing or grinding in a desired time in some cases. is there.

  The present invention has been made in view of such circumstances, and can polish or grind a difficult-to-process substrate such as a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate at a high rate (high polishing or grinding speed), and An object of the present invention is to provide polishing fine particles capable of stably maintaining high polishing quality and a method for producing the same.

  As a result of intensive studies, the inventors of the present invention have found that abrasive particles obtained by irradiating microwave (MW) to a diamond particle having a fullerene derivative attached to the surface of the diamond particle to transform the fullerene derivative into a carbon-containing structure. Was found to be able to process difficult-to-process substrates at a high rate (high polishing or grinding speed) when used for polishing or grinding of difficult-to-process substrates, and completed the present invention.

The present invention has the following configurations.
(1) having diamond particles and a carbon-containing structure derived from a fullerene derivative immobilized on the surface of the diamond particles;
In the Raman spectrum obtained by the light having an excitation wavelength of 532 nm, the maximum intensity of the peaks present in the region of 1300～1350Cm ^-1 derived from the diamond particles and ID, the maximum intensity of the peaks present in the region of 1400～1500Cm ^-1 Is I and the maximum intensity of the peak existing in the region of 1500 to 1650 cm ^-1 is IG, I / ID is 0 or more and less than 0.05, and IG / ID is 0 or more and less than 0.005. Abrasive fine particles (hereinafter sometimes abbreviated as the abrasive fine particles of the present invention).

  (2) In the C1s photoelectron spectrum obtained by surface analysis of the carbon-containing structure using X-ray photoelectron spectroscopy, the maximum intensity in the range of binding energy of 283.8 to 284.2 eV is set to 1 cps, and The abrasive fine particles according to (1), wherein the ratio of 1 cps / second cps is 1.35 or more when the maximum intensity in the energy range of 284.8 to 285.2 eV is set to 2 cps.

(3) The ratio of the absorption peak intensity at 2800 to 3000 cm ⁻¹ in the Fourier transform infrared spectroscopy attributed to carbon-hydrogen stretching vibration is the absorption peak intensity at 3000 to 3600 cm ⁻¹ attributed to oxygen-hydrogen stretching vibration. The abrasive fine particles according to the above (1) or (2), which has a value of 0 or more and 0.5 or less with respect to.

  (4) The abrasive fine particles according to any one of (1) to (3), wherein the carbon-containing structure is present on a part or the whole of the surface of the diamond particles.

  (5) The abrasive fine particles according to any one of (1) to (4), wherein the thickness of the carbon-containing structure is 1 nm or more and 100 nm or less.

(6) the fullerene derivative is a fullerene _{C 60,} wherein (1) to (5) abrasive particles according to any one of.

  (7) The abrasive fine particles according to any one of (1) to (6) above, wherein the average particle diameter of the abrasive fine particles is 0.006 μm or more and 10.1 μm or less.

  (8) The polishing fine particles according to any one of (1) to (7), which are used for polishing or grinding a difficult-to-process substrate.

  (9) The polishing fine particles according to (8), wherein the difficult-to-process substrate is a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate.

(10) A method for producing abrasive fine particles having diamond particles and a carbon-containing structure derived from a fullerene derivative immobilized on the surface of the diamond particles,
Adding and mixing a fullerene derivative in a solution in which the diamond particles are dispersed, and attaching the fullerene derivative to the surface of the diamond particles;
Irradiating the diamond particles to which the fullerene derivative is attached with microwaves to transform the fullerene derivative into a carbon-containing structure, and fixing the carbon-containing structure to the diamond particles. Do
A method for producing abrasive fine particles.

  (11) The method for producing abrasive fine particles according to (10), wherein a main frequency of the microwave is 0.5 GHz or more and 15 GHz or less.

(12) the fullerene derivative is a fullerene _{C 60,} A method of making an abrasive particle according to (10) or (11).

  (13) The method for producing abrasive fine particles according to any one of (10) to (12), wherein the solution is an aqueous solution.

  According to the present invention, polishing or grinding of a difficult-to-process substrate such as a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate can be performed at a high rate (high polishing or grinding speed). It is possible to shorten the manufacturing cost and to reduce the manufacturing cost of a difficult-to-process substrate. Further, by performing polishing or grinding of the substrate with a polishing liquid (polishing slurry) containing the polishing fine particles of the present invention, the projections on the surface of the substrate can be flattened, and the surface roughness (Ra) is improved and the flatness is improved. A substrate having a high polishing quality can be obtained.

FIG. 3 is a spectrum diagram of Fourier transform infrared spectroscopy (FTIR) measurement of the polishing fine particles of Example 1 (the polishing fine particles of the present invention). FIG. 7 is a spectrum diagram of Fourier transform infrared spectroscopy (FTIR) measurement of the polishing fine particles of Comparative Example 2 (polishing fine particles obtained by irradiating ultraviolet (UV) to particles obtained by attaching fullerene hydroxide to the surface of diamond particles). 10 is a transmission electron microscope (TEM) image on a 100 nm scale of the surface of the polishing fine particles of Comparative Example 2 (the polishing fine particles obtained by irradiating ultraviolet (UV) to particles obtained by attaching fullerene hydroxide to the surface of diamond particles). 9 is a 10-nm scale transmission electron microscope (TEM) image of the surface of the polishing fine particles of Comparative Example 2 (the polishing fine particles obtained by irradiating ultraviolet (UV) to particles obtained by attaching fullerene hydroxide to the surface of diamond particles). FIG. 2 is a spectrum diagram of the polishing fine particles of Example 1 (the polishing fine particles of the present invention) measured by Raman spectroscopy. FIG. 9 is a spectrum diagram of the polishing fine particles of Comparative Example 1 (polishing fine particles in which fullerene hydroxide is attached to the surface of diamond particles (not irradiated with microwave (MW) or ultraviolet light (UV))) by Raman spectroscopy. FIG. 9 is a spectrum diagram by Raman spectrometry of the polishing fine particles of Comparative Example 2 (polishing fine particles obtained by irradiating ultraviolet (UV) to particles obtained by attaching fullerene hydroxide to the surface of diamond particles). FIG. 2 is a spectrum diagram of the abrasive fine particles of Example 1 (the abrasive fine particles of the present invention) measured by X-ray photoelectron spectroscopy (XPS). Spectrum of X-ray photoelectron spectroscopy (XPS) measurement of the polishing fine particles of Comparative Example 1 (the polishing fine particles having fullerene hydroxide adhered to the surface of diamond particles (not irradiated with microwave (MW) or ultraviolet (UV))) FIG. Polishing liquid (polishing slurry) containing polishing fine particles consisting only of diamond particles, polishing liquid (polishing slurry) obtained in Example 1, polishing liquid (polishing slurry) obtained in Comparative Example 1, or Comparative Example 2 It is a figure which shows the result of MRR (material removal rate) in the case of using the obtained polishing liquid (polishing slurry). FIG. 5 is a diagram showing a surface image (magnification of an objective lens: 20 times) of a sapphire wafer after polishing (second time) when a polishing liquid (polishing slurry) containing polishing fine particles consisting only of diamond particles is used. FIG. 3 is a diagram showing a surface image (magnification of an objective lens: 20 times) of a sapphire wafer after polishing (second time) when the polishing liquid (polishing slurry) obtained in Example 1 is used. FIG. 9 is a view showing a surface image (magnification of an objective lens: 20 times) of a sapphire wafer after polishing (second time) when the polishing liquid (polishing slurry) obtained in Comparative Example 1 is used. FIG. 9 is a view showing an image (magnification of an objective lens: 20 times) of a sapphire wafer surface after polishing (second time) when the polishing liquid (polishing slurry) obtained in Comparative Example 2 is used.

-Abrasive fine particles of the present invention-
The abrasive fine particles of the present invention are characterized by having diamond particles and a carbon-containing structure derived from a fullerene derivative immobilized on the surface of the diamond particles.

  The diamond particles according to the present invention may be either primary particles or aggregates (secondary particles) obtained by aggregating the primary particles as long as the particles are particulate. Among these particles, primary particles are preferred.

  The average particle diameter of the diamond particles according to the present invention is, for example, usually from 0.005 μm to 10 μm, preferably from 0.05 μm to 6 μm, more preferably from 0.05 μm to 2 μm, and more preferably from 0.1 μm to 1. Particularly preferred is 2 μm or less. Here, the “average particle size” refers to a mode (mode size) of a number-based particle size frequency distribution curve measured by a laser diffraction method or the like.

Examples of the fullerene derivative according to the present invention include fullerene C ₆₀ , fullerene C ₇₀ , fullerene hydroxide C ₆₀ , fullerene hydroxide C ₇₀ , hydrogenated fullerene C ₆₀ , hydrogenated fullerene C ₇₀ , fullerene soot, onion-like carbon, and the like. Is mentioned. Among these fullerene derivatives, preferably hydroxylated fullerene C ₆₀ and fullerene C _70, readily available, and, in terms of high dispersibility in water, fullerene C ₆₀ is more preferable.

  The carbon-containing structure according to the present invention is one that is immobilized on the surface of the above-described diamond particles and is derived from the above-described fullerene derivative. That is, the carbon-containing structure is deteriorated by, for example, irradiating microwaves (MW) to the diamond particles having the surface of the diamond particles to which the fullerene derivative is adhered under the conditions described below to chemically bond the fullerene derivatives to each other. It is formed by this.

  The carbon-containing structure according to the present invention may be present on a part of the surface of the diamond particle, or may be present on the entire surface of the diamond particle. It is preferable to cover a part or all of the surface.

  The thickness of the carbon-containing structure according to the present invention is generally from 1 nm to 100 nm, preferably from 1 nm to 20 nm, more preferably from 1 nm to 10 nm. Here, the thickness of the carbon-containing structure may be measured by, for example, a transmission electron microscope (TEM).

  The abrasive fine particles of the present invention having such a shape have the following characteristics.

That is, the abrasive fine particles of the present invention have a maximum intensity of a peak existing in a region of 1300 to 1350 cm ⁻¹ derived from diamond particles in a Raman spectrum obtained with light having an excitation wavelength of 532 nm as ID, and a peak intensity of 1400 to 1500 cm ⁻¹ . When the maximum intensity of the peak existing in the region is I and the maximum intensity of the peak existing in the region of 1500 to 1650 cm ^-1 is IG, I / ID is 0 or more and less than 0.05, and IG / ID is 0 or more and less than 0.005. In a Raman spectrum obtained by Raman spectroscopy using light having an excitation wavelength of 532 nm, a Raman shift existing in a region of 1300 to 1350 cm ⁻¹ is a peak derived from diamond and is called a D peak. In a Raman spectrum obtained by Raman spectroscopy, a Raman shift existing in a region of 1500 to 1650 cm ⁻¹ is a peak derived from graphene or graphene-like carbon and is called a G peak. That is, the polishing particles of the present invention, with respect to D peak derived from the diamond particles present in the region of 1300～1350Cm ^-1, and peaks present in the region of 1400～1500Cm ^-1, in the region of 1500～1650Cm ^-1 It is characterized in that almost no G peaks derived from graphene or graphene-like carbon exist or are below the detection limit.

  Examples of the light having an excitation wavelength of 532 nm include a semiconductor laser light.

  The Raman spectrum may be measured, for example, by placing the abrasive fine particles of the present invention on a slide glass and using a Raman spectrometer (for example, “MicroRAM-300” manufactured by Lambda Vision Co., Ltd.). When the polishing particles of the present invention are present in a solution, for example, the solution (polishing liquid / polishing slurry) is dropped into an arbitrary container, and after removing water with a vacuum drier or the like, the water is removed. What has removed the abrasive fine particles from the container may be used for the measurement.

In the present invention, 1300～1350Cm maximum intensity of the D peak derived from the diamond particles present in the region of ^-1; regions I and 1500~1650cm ^-1; ID, the maximum intensity of the peaks present in the region of 1400～1500Cm ^-1 Is the maximum intensity of the G peak derived from graphene or graphene-like carbon; IG means a value obtained by the following method. That is, for the peaks of the components A to C in the Raman spectrum obtained using a Raman spectrometer (laser Raman spectrophotometer, excitation wavelength: 532 nm), the maximum intensity is obtained from the baseline of each component.
Component A: wave number; 1300 to 1350 cm ^-1 region: D peak, half width; 4 to 16 cm ^-1
Component B: wavenumber; region of 1400~1500cm ^-1, the half width; 40～120Cm ^-1
Component C: wave number; region of 1500 to 1650 cm ^-1 : G peak, half width; 40 to 120 cm ^-1
The base line of each component is a straight line connecting the following two intensity values.
Baseline components A: 1295 ^-1 of intensity values and 1360 cm ^-1 of the base of the linear component B that connects the two points of the intensity value line: connecting two points of the intensity values of the intensity values and 1600 cm ^-1 of 1354Cm ^-1 it linear component C baseline: the maximum intensity of the linear components that connects two points of the intensity values of 1470 cm ^-1 of the intensity values and 1680 cm ^-1, the intensity values in wavenumber region of each component and (Y value), the The difference (Y value−Z value) between the intensity value (Z value) at the intersection of the perpendicular line drawn on the Raman shift axis and the baseline is determined from the intensity value, and the value with the largest value is defined as the maximum intensity. Taking the maximum intensity of the component A as an example, the difference between the Y value of the component A and the Z value of the component A is determined, and the value having the largest numerical value among the obtained intensity values is defined as the maximum intensity of the component A. .
Maximum intensity of the component A: wavenumber; of the intensity values obtained in the region of 1300～1350Cm ^-1, value is the maximum intensity of the largest value component B: wavenumber; 1400～1500Cm resulting intensity values in the region of ^-1 Among the intensity values obtained in the range of 1500 to 1650 cm ^-1 , the largest value of the value component C having the largest numerical value among the values:

The maximum intensity of each component is determined, and the maximum intensity of the component A is defined as the maximum intensity of a D peak derived from diamond particles existing in a region of 1300 to 1350 cm ^-1 ; ID, and the maximum intensity of the component B is set at 1400 to 1500 cm ^-1. The maximum intensity of the peak existing in the region of I; I and the maximum intensity of the component C as the maximum intensity of the G peak derived from graphene or graphene-like carbon existing in the region of 1500 to 1650 cm ^-1 ; IG.

  From the maximum intensity of the peak of each component obtained in this manner, the maximum intensity of component A (D peak); the maximum intensity of component B with respect to ID; the ratio of I: I / ID, and the ratio of component A (D peak) Maximum intensity; maximum intensity of component C (G peak) to ID; ratio of IG: IG / ID is determined.

  When both I / ID and IG / ID are obtained by the above method, the abrasive fine particles of the present invention have an I / ID of 0 or more and less than 0.05, and an IG / ID of 0 or more and less than 0.005. There is a feature that there is.

  In the polishing fine particles of the present invention, the I / ID is preferably 0 or more and less than 0.03, more preferably 0 or more and less than 0.02, further preferably 0 or more and less than 0.01, It is particularly preferable that it is 0 or more and less than 0.005.

  In the abrasive fine particles of the present invention, IG / ID is preferably 0 or more and less than 0.004, more preferably 0 or more and less than 0.003, and further preferably 0 or more and 0.0024 or less.

  In the abrasive fine particles of the present invention, as a combination of I / ID and IG / ID, it is preferable that I / ID is 0 or more and less than 0.03, and IG / ID is 0 or more and less than 0.004. .

  The abrasive fine particles of the present invention preferably have the following characteristics.

  The abrasive fine particles of the present invention have a maximum intensity in a C1s photoelectron spectrum obtained by surface analysis of a carbon-containing structure using X-ray photoelectron spectroscopy (XPS) in a binding energy range of 283.8 to 284.2 eV. Is the first cps, and when the maximum intensity within the binding energy range of 284.8 to 285.2 eV is the second cps, the first cps / second cps is preferably 1.35 or more. The polishing fine particles of the present invention have a binding energy having a peak in the range of 283.8 to 284.2 eV in the C1s photoelectron spectrum obtained by surface analysis of the carbon-containing structure using X-ray photoelectron spectroscopy (XPS). The maximum intensity of the peak is 1.35 times or more the maximum intensity of the peak in the range of 284.8 to 285.2 eV based on the binding energy of the C-OH bond derived from the fullerene derivative. It is preferable to have Although the upper limit of the first cps / second cps is not particularly limited, it is, for example, usually 5.0 or less, preferably 3.0 or less.

  In the abrasive fine particles of the present invention, the first cps / second cps is preferably 1.40 or more, more preferably 1.45 or more, further preferably 1.50 or more, and still more preferably 1.70 or more. Is particularly preferred.

The measurement of X-ray photoelectron spectroscopy may be performed, for example, as follows.
After the target abrasive particles of the present invention are dispersed in water such as ion-exchanged water, the resulting dispersion is dispersed with a shaker such as a reciprocating shaker “SR-2RSS” (manufactured by Taitec Co., Ltd.). Get. Next, the dispersion liquid is centrifuged at an appropriate rotation speed (for example, rotation speed of 2,200 rpm) for several minutes using a centrifuge such as a table top centrifuge “4000” (manufactured by Kubota Shoji Co., Ltd.), and then supernatant is removed. The liquid is removed, and ion-exchanged water is added to the precipitate to disperse it. This operation was repeated several times, and it was visually confirmed that the supernatant liquid after centrifugation became clear. Thereafter, 200 μL of the dispersion liquid is dropped on the thermal oxide film wafer, and X-ray photoelectron spectroscopy is performed on the measurement target portion of the polishing fine particles after air drying. In the measurement of X-ray photoelectron spectroscopy, X2 photoelectron spectroscopy was used to measure Si2p in the measurement target portion of the polishing fine particles, and it was confirmed that no Si2p spectrum was obtained. It is desirable to perform the above-mentioned analysis in a state where it is deposited on the surface.
The XPS measurement may be performed, for example, under the following conditions.
X-ray photoelectron spectrometer: Scanning dual X-ray photoelectron spectrometer PHI Quantes [manufactured by ULVAC-PHI, Inc.]
Excitation source: mono. AIKα, 10 μm ² , 25 W, 15 kV
Analysis size: Elliptical photoelectron extraction angle of about 1 mm: 0 °
Sample stage tilt: 45 °
Capture area
Narrow Scan: Si2p (110 to 95 ev), C1s (290 to 280 eV)
Pass Energy: 69

  Further, the abrasive fine particles of the present invention preferably have the following characteristics.

The abrasive fine particles of the present invention have a ratio of the absorption peak intensity at 2800 to 3000 cm ⁻¹ in the Fourier transform infrared spectroscopy (FTIR) spectrum attributed to the carbon-hydrogen stretching vibration of 3000 to 8000 attributable to the oxygen-hydrogen stretching vibration. More preferably, it is 0 or more and 0.5 or less with respect to the absorption peak intensity at 3600 cm ^-1 . The abrasive fine particles of the present invention have an absorption peak intensity of 2800 to 3000 cm ⁻¹ in a Fourier transform infrared spectroscopy (FTIR) spectrum attributed to carbon-hydrogen stretching vibration, and have an absorption peak intensity of 3,000 to 8000 belonging to oxygen-hydrogen stretching vibration. It is more preferable that the absorption peak intensity at 3600 cm ^-1 is hardly confirmed or that the absorption peak intensity is smaller.

Fourier transform infrared spectroscopy (FTIR) can be measured, for example, by mixing the abrasive fine particles of the present invention with potassium bromide and crushing in a mortar, collecting the obtained powder in a microtablet forming device or the like, and performing Fourier transform red It may be performed using an external spectrometer. When the polishing particles of the present invention are present in a solution, for example, the solution (polishing liquid / polishing slurry) is dropped into an arbitrary container, and after removing water with a vacuum drier or the like, the water is removed. What has removed the abrasive fine particles from the container may be used for the measurement.
The Fourier transform infrared spectroscopy may be performed, for example, under the following conditions.
Fourier transform infrared spectrometer: FT / IR-615 [manufactured by JASCO Corporation]
Measuring method: Transmission method total number of times: 16 times

  The abrasive fine particles of the present invention thus obtained may be either primary particles or aggregates (secondary particles) in which the primary particles are aggregated, and are not particularly limited.

  The average particle diameter of the abrasive fine particles of the present invention is, for example, usually from 0.006 μm to 10.1 μm, preferably from 0.051 μm to 6.1 μm, more preferably from 0.051 μm to 2.02 μm, and Particularly preferred is a range of. Here, the “average particle size” refers to a mode (mode size) of a number-based particle size frequency distribution curve measured by a laser diffraction method or the like.

-Method for producing abrasive fine particles of the present invention-
The abrasive fine particles of the present invention are prepared by adding a fullerene derivative to a solution in which diamond particles are dispersed, mixing and adding the fullerene derivative to the surface of the diamond particles (first step),
Next, the above-mentioned diamond particles to which the fullerene derivative is attached are irradiated with microwaves (MW) to convert the fullerene derivative into a carbon-containing structure, thereby immobilizing the carbon-containing structure on the diamond particles (No. 2 steps).

  Examples of the diamond particles in the method for producing abrasive fine particles of the present invention include diamond particles having the same average particle diameter as the diamond particles in the abrasive fine particles of the present invention. In addition, examples of the fullerene derivative in the method for producing abrasive fine particles of the present invention include those similar to the fullerene derivative in the abrasive fine particles of the present invention.

The detailed procedure of the method for producing abrasive fine particles of the present invention will be described below.
First, 5 mg to 1.5 g of the above diamond particles are added to 50 to 500 mL of a solvent, and the diamond particles are dispersed using, for example, a disperser. Next, 5 mg to 1.5 g of the fullerene derivative is added to the obtained dispersion of diamond particles, and the fullerene derivative is attached to the surface of the diamond particles (first step).
Next, the diamond particles to which the fullerene derivative is attached are irradiated with microwaves (MW) to transform the fullerene derivative into a carbon-containing structure by, for example, chemically bonding each other. By fixing the containing structure (second step), the abrasive fine particles of the present invention can be produced.

  The amount of the diamond particles to be added in the production method of the present invention is, for example, that the concentration of the diamond particles in the solution is, for example, generally 0.01% by mass to 0.3% by mass, preferably 0.03% by mass to 0.3% by mass. It is desirable to add so as to be 2% by mass or less, more preferably 0.05% by mass or more and 0.15% by mass or less.

  The solvent for dispersing the diamond particles is not particularly limited as long as the solvent does not dissolve or corrode a CMP pad such as a polyurethane pad and can disperse the diamond particles. Specific examples of such a solvent include, for example, water such as ion-exchanged water, purified water, and ultrapure water; for example, an alcoholic solvent such as methanol, ethanol, and propanol; and an aromatic hydrocarbon such as toluene and xylene. Ketone solvents such as 2-propanone (acetone), 2-butanone (ethyl methyl ketone) and 4-methyl-2-pentanone (methyl isobutyl ketone); for example, diethyl ether, diisopropyl ether, tetrahydrofuran, 1 And ether solvents such as 4-dioxane; for example, amide solvents such as N, N-dimethylformamide, N, N-dimethylacetamide, 1-methyl-2-pyrrolidinone (N-methylpyrrolidone). These solvents may be used alone or in combination of two or more.

  Among these solvents, water such as ion-exchanged water, purified water, and ultrapure water; and alcoholic solvents such as methanol, ethanol, and propanol are preferable, and water such as ion-exchanged water, purified water, and ultrapure water are more preferable. preferable.

  The use amount of the above-mentioned solvent is, for example, usually 50 mL or more and 500 mL or less, preferably 100 mL or more and 300 mL or less, and more preferably 150 mL or more and 250 mL or less.

  It is desirable to add a basic substance to the dispersion of the diamond particles in order to enhance the dispersibility of the diamond particles and to increase the solubility or dispersibility of the fullerene derivative.

  Examples of the basic substance include alkali metal hydroxides such as sodium hydroxide, potassium hydroxide, and lithium hydroxide; for example, tetramethylammonium hydroxide, tetraethylammonium hydroxide, tetrapropylammonium hydroxide, tetrabutyl Quaternary ammonium salts such as ammonium hydroxide and (hydroxyethyl) trimethylammonium hydroxide [choline]; for example, monoethanolamine, diethanolamine, triethanolamine, monoisopropanolamine, tris (hydroxymethyl) aminomethane, 2- ( (Morpholino) alkanolamines such as ethanol. In addition, these basic compounds may be used alone or in combination of two or more basic compounds.

  The amount of the basic compound used is such that the pH of the solution after the addition of the basic compound is, for example, usually 8 to 14, preferably 9 to 13, and more preferably 10.5 to 12.5. It is desirable to add

  Further, a dispersant or a surfactant generally used in this field may be added to the above-mentioned dispersion liquid.

  The addition amount of the fullerene derivative according to the production method of the present invention is such that the concentration of the fullerene derivative in the solution is, for example, usually from 0.05% by mass to 0.2% by mass, and preferably from 0.05% by mass to 0.2% by mass. It is desirable to add so as to be 18% by mass or less, more preferably 0.05% by mass or more and 0.15% by mass or less, further preferably 0.07% by mass or more and 0.12% by mass or less.

  The temperature at which the fullerene derivative is attached to the surface of the diamond particles is, for example, usually -20 ° C to 80 ° C, preferably 0 ° C to 60 ° C, more preferably 5 ° C to 40 ° C, and more preferably 10 ° C or more. Particularly preferred is 35 ° C. or lower.

  The time for attaching the fullerene derivative to the surface of the diamond particles is, for example, usually 0.05 hours to 24 hours, preferably 0.1 hours to 12 hours, more preferably 0.5 hours to 6 hours. preferable. In addition, regardless of the dispersion state of the diamond particles, the fullerene derivative can be attached to the surface of the diamond particles after the above-mentioned time has elapsed, regardless of the dispersion state of the diamond particles. Alternatively, the solution may be appropriately stirred, and among them, it is preferable to stir the solution.

  The first step according to the production method of the present invention does not necessarily need to be performed under the above-described conditions. However, if the first step is performed under the above-described conditions, the (fullerene derivative adheres) in a simple, accurate, and desirable mode. ) Diamond particles can be obtained.

  As a microwave for irradiating the diamond particles with a microwave (MW), a microwave whose main wavelength is, for example, usually 0.5 GHz or more and 15 GHz or less, and preferably 0.8 GHz or more and 3 GHz or less is preferable, and 1 GHz or more. Microwaves below 3 GHz are more preferred. Note that microwave irradiation may be performed using a microwave irradiation apparatus usually used in this field.

  The irradiation intensity when irradiating the diamond particles with microwaves (MW) is, for example, usually from 30 W to 200 W, preferably from 50 W to 150 W, more preferably from 80 W to 120 W.

  The irradiation time when irradiating the diamond particles with microwaves (MW) is, for example, usually from 10 to 300 seconds, preferably from 30 to 150 seconds, more preferably from 60 to 120 seconds.

  The second step according to the production method of the present invention does not necessarily need to be performed under the above-described conditions. However, if the second step is performed under the above-described conditions, the polishing fine particles of the present invention can be easily and accurately obtained in a desirable mode. Obtainable.

  The thus obtained polishing fine particles of the present invention can be used as an abrasive (abrasive) of a polishing liquid (polishing slurry). As the polishing liquid (polishing slurry), the solution immediately after the production of the polishing fine particles of the present invention is separated into the polishing fine particles of the present invention and a solvent by a centrifuge or the like, and the polishing fine particles of the present invention are taken out. The polishing liquid (polishing slurry) may be dispersed in the polishing solution or the like, or the solution immediately after the production obtained in the production process of the polishing fine particles of the present invention may be used as it is as the polishing liquid (polishing slurry). The centrifuge used for the above-mentioned separation operation may be a centrifuge usually used in this field.

  The solution immediately after the production of the abrasive fine particles of the present invention is separated into the abrasive fine particles of the present invention and a solvent by a centrifugal separator or the like, and the abrasive fine particles of the present invention are taken out. The abrasive particles of the invention may be washed.

  In producing the above-mentioned polishing liquid (polishing slurry), the polishing fine particles of the present invention are mixed with water so that the mass of the polishing fine particles of the present invention in the solution is 0.05% by mass or more and 0.15% by mass or less. It is desirable to disperse in a solvent such as

  The above-mentioned polishing liquid (polishing slurry) usually contains, for example, a polyphosphoric acid-based dispersant such as phytin, a dispersant such as a silicon-based dispersant, for example, a viscosity modifier such as ethylene glycol, and a surfactant. May be used in combination with additives and polishing aids generally used.

  The abrasive fine particles of the present invention are used in a polishing liquid (polishing slurry) as an abrasive (abrasive) for polishing (eg, CMP) or grinding a difficult-to-process substrate such as a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate. In addition, not only can these difficult-to-process substrates be processed at a high rate (high polishing or grinding speed), but also the projections on the substrate surface can be flattened, the surface roughness (Ra) can be improved, and a substrate having a high flatness can be obtained. Can be obtained.

  Hereinafter, the present invention will be specifically described based on examples and comparative examples, but the present invention is not limited to these examples.

Example 1 Preparation of Polished Fine Particles Having Carbon-Containing Structure by Microwave (MW) Diamond particles having an average particle diameter of 1 μm (1000 nm) were added to 200 mL of an aqueous solution adjusted to pH 12 with potassium hydroxide at room temperature. 200 mg of “Hyprez 1-STD-MA” manufactured by the company was dispersed. Fullerene hydroxide [manufactured by Frontier Carbon Co., Ltd.] was added to the dispersion so that the concentration of the fullerene hydroxide in the dispersion was 0.1% by mass, and the mixture was stirred for 60 minutes to form a hydroxide on the surface of the diamond particles. Fullerene was deposited. Next, a predetermined amount of the dispersion liquid of the diamond particles to which the fullerene hydroxide is adhered is fractionated, and is subjected to microwave (MW) irradiation using a microwave (MW) irradiator [“Green Motif Ib / II” manufactured by IDX Corporation]. (Wavelength: 135 nm, pulse frequency: 2.45 GHz, irradiation intensity: 100 W) for 90 seconds to change the fullerene hydroxide adhering to the surface of the diamond particles into a carbon-containing structure, thereby obtaining the abrasive fine particles of the present invention. (Polishing slurry of 1.0% by mass) was obtained. The Fourier transform infrared spectroscopy (FTIR) spectrum of the obtained abrasive fine particles was measured under the following conditions. The result is shown in FIG.
<Measurement conditions>
Fourier transform infrared spectrometer: FT / IR-615 [manufactured by JASCO Corporation]
Measuring method: Transmission method total number of times: 16 times

Comparative Example 1: Preparation of Abrasive Fine Particles without Carbon-Containing Structure At room temperature, 200 mL of an aqueous solution adjusted to pH 12 with potassium hydroxide was mixed with diamond particles having an average particle size of 1 μm (1000 nm) (“Hyprez” manufactured by Engis Corporation) at room temperature. 1-STD-MA ") 200 mg was dispersed. Fullerene hydroxide [manufactured by Frontier Carbon Co., Ltd.] was added to the dispersion so that the concentration of the fullerene hydroxide in the dispersion was 0.1% by mass, and the mixture was stirred for 60 minutes to form a hydroxide on the surface of the diamond particles. A polishing liquid containing abrasive fine particles for comparison [abrasive fine particles in which fullerene hydroxide is adhered to the surface of diamond particles (not irradiated with microwave (MW) or ultraviolet (UV)) by adhering fullerenes] (1.0 mass% polishing slurry) was obtained.

Comparative Example 2: Preparation of Polished Fine Particles Having Carbon-Containing Structure by Ultraviolet (UV) Diamond particles having an average particle diameter of 1 μm (1000 nm) (Engis Co., Ltd.) were added at room temperature to 200 mL of an aqueous solution adjusted to pH 12 with potassium hydroxide. 200 mg of “Hyprez 1-STD-MA” manufactured by the company was dispersed. Fullerene hydroxide [manufactured by Frontier Carbon Co., Ltd.] was added to the dispersion so that the concentration of the fullerene hydroxide in the dispersion was 0.1% by mass, and the mixture was stirred for 60 minutes to form a hydroxide on the surface of the diamond particles. Fullerene was deposited. Next, a predetermined amount of the dispersion liquid of the diamond particles to which the fullerene hydroxide is adhered is fractionated, and an ultraviolet (UV) irradiator [Spectrum Physics Co., Ltd. "LD excitation Q switch solid laser"] (Wavelength: 355 nm, pulse frequency: 50 kHz, irradiation intensity: 270 mW) for 60 minutes, and polishing fine particles for comparison [polishing by irradiating ultraviolet (UV) to particles in which fullerene hydroxide is adhered to the surface of diamond particles] (Fine particles) was obtained (a polishing slurry of 1.0% by mass). The Fourier transform infrared spectroscopy (FTIR) spectrum of the obtained abrasive fine particles was measured under the following conditions. The result is shown in FIG. FIG. 3 shows a transmission electron microscope (TEM) image of the obtained polishing fine particles on a 100 nm scale, and FIG. 4 shows a transmission electron microscope (TEM) image of the polishing fine particles on a 10 nm scale.
<Measurement conditions>
Fourier transform infrared spectrometer: FT / IR-615 [manufactured by JASCO Corporation]
Measuring method: Transmission method total number of times: 16 times

Experimental Examples 1 to 3: Raman spectroscopic measurement of abrasive fine particles The polishing slurries obtained in Example 1 and Comparative Examples 1 and 2 were each dropped on a plastic tray, and after removing water with a vacuum dryer, the polishing slurry was removed from the plastic tray. The Raman spectrum of the abrasive fine particles taken out on the slide glass was measured under the following conditions.
<Measurement conditions>
Raman spectrometer: Lambda Vision “MicroRAM-300”
Detector: "CI0151" manufactured by Hamamatsu Photonics KK
Excitation light source: Semiconductor laser Excitation wavelength: 532 nm
Laser output: 30mW
Beam diameter (reference value at each magnification): 5 μm (× 50)
Integrated time: 10sec (1sec x 10 times)
In the Raman spectrum measured under the above conditions, for the following three components A to C in the range of 1200 to 1750 cm ⁻¹ , the maximum intensity was determined from the baseline of each component. The base line of each component was a straight line connecting the following two intensity values.
Baseline components A: 1295 ^-1 of intensity values and 1360 cm ^-1 of the base of the linear component B that connects the two points of the intensity value line: connecting two points of the intensity values of the intensity values and 1600 cm ^-1 of 1354Cm ^-1 linear component C baseline: the maximum intensity of the linear components that connects two points of the intensity values of the intensity values and 1680 cm ^-1 in 1470 cm ^-1, the intensity values in the following wavenumber region of each component and (Y value) Then, the difference (Y value−Z value) between the intensity value (Z value) at the intersection of the perpendicular line drawn on the Raman shift axis and the baseline from the intensity value was determined, and the value with the largest numerical value was defined as the maximum intensity. Table 1 shows the results. Further, I / ID and IG / ID of each of the polished fine particles of Example 1 and Comparative Examples 1 and 2 were determined based on the maximum strengths of the obtained components A to C. The results are shown in Table 1. Further, FIG. 5 shows a spectrum diagram of the polishing fine particles of Example 1 (polishing fine particles having a carbon-containing structure by microwave (MW): the polishing fine particles of the present invention) measured by Raman spectroscopy. FIG. 6 is a spectrum diagram by Raman spectrometry of the polishing fine particles having no containing structure), and FIG. 6 is a spectrum diagram by Raman spectrometry of the polishing fine particles (polishing fine particles having the carbon-containing structure by ultraviolet (UV)) of Comparative Example 2. Are shown in FIG.
Component A: wave number; 1300 to 1350 cm ^-1 region: D peak, half width; 4 to 16 cm ^-1
Component B: wavenumber; region of 1400~1500cm ^-1, the half width; 40～120Cm ^-1
Component C: wave number; region of 1500 to 1650 cm ^-1 : G peak, half width; 40 to 120 cm ^-1
Maximum intensity of component A: wave number; value having the largest numerical value among intensity values obtained in an area of 1300 to 1350 cm ^-1 ; ID
Maximum intensity of component B: wave number; value having the largest numerical value among intensity values obtained in the region of 1400 to 1500 cm ^-1 ; I
Maximum intensity of component C: wave number; value with the largest numerical value among intensity values obtained in a region of 1500 to 1650 cm ^-1 ; IG

Experimental Examples 4 to 5: X-ray Photoelectron Spectroscopy (XPS) Measurement of Polished Fine Particles The polishing slurries obtained in Example 1 and Comparative Example 1 were dispersed using a reciprocating shaker “SR-2RSS” (manufactured by Taitec Corporation). After that, the dispersion was centrifuged at 2,200 rpm for 15 minutes using a table-top centrifuge "4000" (manufactured by Kubota Corporation), the supernatant was removed, and ion-exchanged water was added to the sediment. , And the operation of centrifuging the mixture was repeated three times. After visually confirming that the supernatant liquid after centrifugation three times became clear, 200 μL of the dispersion liquid was dropped on the thermal oxide film wafer, and the measurement target portion of the abrasive fine particles after air drying was subjected to the following. X-ray photoelectron spectroscopy was performed under the following conditions. In the measurement of X-ray photoelectron spectroscopy, a sufficient amount of the polishing fine particles was deposited on the wafer because the Si2p spectrum was not obtained by measuring Si2p in the measurement target portion of the polishing fine particles with an X-ray photoelectron spectroscopy analyzer. The test was carried out in a state where it was deposited.
<Measurement conditions>
X-ray photoelectron spectrometer: Scanning dual X-ray photoelectron spectrometer PHI Quantes [manufactured by ULVAC-PHI, Inc.]
Excitation source: mono. AIKα, 10 μm ² , 25 W, 15 kV
Analysis size: Elliptical photoelectron extraction angle of about 1 mm: 0 °
Sample stage tilt: 45 °
Capture area
Narrow Scan: Si2p (110 to 95 ev), C1s (290 to 280 eV)
Pass Energy: 69

  The intensity at each binding energy in the photoelectron spectrum of C1s was determined at intervals of 0.1 eV by X-ray photoelectron spectroscopy (XPS) measurement. Table 2 shows the intensity at a binding energy of 283.8 to 284.2 eV and the intensity at a binding energy of 284.8 to 285.2 eV. Further, based on the obtained intensities, the first cps (maximum intensity in a binding energy range of 283.8 to 284.2 eV) and the second cps (binding energy) of the respective polishing fine particles of Example 1 and Comparative Example 1 were obtained. (The maximum intensity in the range of 284.8 to 285.2 eV) was selected, and the first cps / second cps was determined based on these. Further, FIG. 8 shows a spectrum diagram of the polishing fine particles of Example 1 (polishing fine particles having a carbon-containing structure by microwave (MW): the polishing fine particles of the present invention) measured by X-ray photoelectron spectroscopy (XPS), and Comparative Example 1 X-ray photoelectron spectroscopy (XPS) measurement of the abrasive fine particles (abrasive fine particles having no carbon-containing structure) is shown in FIG.

Experimental Example 6: Evaluation of MRR of polishing fine particles Diamond particles were dispersed in water such that the mass of the diamond particles in the solution was 0.13% by mass, and the polishing particles contained only the diamond particles. A polishing liquid (polishing slurry) was prepared and used for evaluation. The polishing liquid (polishing slurry) obtained in Example 1 and the polishing liquid (polishing slurry) obtained in Comparative Examples 1 and 2 were used for evaluation as they were.
Next, chemical mechanical polishing (CMP) is performed on the sapphire wafer that has been subjected to rough polishing in advance under the following conditions, and the material removal rate per hour (according to the following formulas (1) and (2)) Material removal rate (MRR) was calculated for each polishing slurry. The results are shown in Table 3 and FIG.
<Polishing conditions>
Polishing device: Desktop type single-side polishing device DIA LAP ACE ML-160A (Malto Co., Ltd.)
Polishing pad: SUBA 600 (made by Anchor Techno Co., Ltd.)
Polishing pressure: 45.9 kPa (6.6 psi)
Platen rotation speed: 60 rotations / minute Head rotation speed: 60 rotations / minute Polishing time: 1 hour Supply rate of polishing liquid (polishing slurry): 0.3 mL / minute (flowing)
Polishing liquid temperature: 25 ° C
Polishing object: Sapphire wafer (conductivity type: A type)
Area to be polished: 113.04 mm ²
<Calculation formula>
(1) white polished up [cm] = the mass difference before and after polishing of the sapphire wafer [g] / density of the sapphire wafer ^{[g / cm 3] (=} 3.98g / cm 3) / polished area ^[cm 2] (= 113.04 mm ² )
(2) Polishing rate [μm / hour] = polishing margin [cm] × 10 ⁴ / polishing time (1 hour)

As is clear from the results of Table 3 and FIG. 10, when the polishing fine particles (polishing slurry) of the present invention of Example 1 were used, the polishing fine particles (polishing slurry) consisting only of diamond particles and the polishing fine particles of Comparative Example 1 were used. It was found that the MRR was more than twice as high as that in the case of using the polishing fine particles (polishing slurry). Further, it was found that the MRR was higher when the polishing fine particles (polishing slurry) of Example 1 of the present invention were used than when the polishing fine particles (polishing slurry) of Comparative Example 2 were used.
The MRR when the polishing fine particles (polishing slurry) of the present invention of Example 1 are used and the polishing fine particles (polishing slurry) of Comparative Example 1 to which neither the microwave (MW) nor the ultraviolet light (UV) is irradiated. Are different from each other, it is suggested that the irradiation of microwaves (MW) alters the fullerene hydroxide attached to the surface of the diamond particles due to chemical bonding and the like. Furthermore, since the MRR when using the polishing fine particles (polishing slurry) of the present invention of Example 1 and the MRR when using the polishing fine particles (polishing slurry) irradiated with ultraviolet rays (UV) of Comparative Example 2 are different, Suggests that the carbon-containing structure caused by the alteration of the fullerene hydroxide by microwave irradiation is different from the structure caused by the alteration of the fullerene hydroxide by ultraviolet (UV) irradiation Is done.

Experimental Example 7 Evaluation of Ra of Polished Fine Particles Diamond particles were dispersed in water such that the mass of the diamond particles in the solution was 0.13% by mass, and contained abrasive fine particles consisting of diamond particles only. A polishing liquid (polishing slurry) was prepared and used for evaluation. The polishing liquid (polishing slurry) obtained in Example 1 and the polishing liquid (polishing slurry) obtained in Comparative Examples 1 and 2 were used for evaluation as they were.
Next, the sapphire wafer, which has been subjected to rough polishing in advance to have a uniform surface roughness, is subjected to chemical mechanical polishing (CMP) under the following conditions, and polished using an atomic force microscope (AFM). The surface roughness (Ra) of the wafer was measured. Incidentally, when the measurement of Ra, was ground twice with each polishing liquid (abrasive slurry), and performs the measurement in the range of 500 nm ² at any three locations for each wafer after polishing, the average value Was defined as Ra. Table 4 shows the results. FIG. 11 shows the surface image (magnification of the objective lens: 20 times) of the sapphire wafer after polishing (second time) in the case of using polishing fine particles (polishing slurry) consisting only of diamond particles. FIG. 12 shows the surface image of the sapphire wafer after polishing (second time) (magnification of the objective lens: 20 times) when the polishing fine particles (polishing slurry) were used, and the polishing fine particles (polishing slurry) of Comparative Example 1 were used. FIG. 13 shows the surface image (magnification of the objective lens: 20 times) of the sapphire wafer after polishing (second time) in the case where the polishing was performed (second time), and after polishing (second time) in the case where the polishing fine particles (polishing slurry) of Comparative Example 2 were used. FIG. 14 shows the surface image (magnification of the objective lens: 20 times) of the sapphire wafer of FIG.
<Polishing conditions>
Polishing equipment: “Desktop single-side polishing machine DIA LAP ACE ML-160A” manufactured by Maruto Co., Ltd.
Polishing pad: "SUBA 600" manufactured by Anchor Techno Co., Ltd.
Polishing pressure: 45.9 kPa (6.6 psi)
Platen rotation speed: 60 rotations / minute Head rotation speed: 60 rotations / minute Polishing time: 1 hour Supply rate of polishing liquid (polishing slurry): 0.3 mL / minute (flowing)
Polishing liquid temperature: 25 ° C
Polishing object: Sapphire wafer (conductivity type: A type)
Area to be polished: 113.04 mm ²
<Ra measurement conditions>
Atomic force microscope: SPA-300V (manufactured by Seiko Instruments Inc.)
Cantilever: POINTPROVE-PLUS Silicon-SPM-Sensor PPP-cont-20

  As is clear from the results in Table 4, when the polishing fine particles (polishing slurry) of the present invention of Example 1 were used in the surface polishing of the wafer, the polishing fine particles (polishing slurry) consisting only of diamond particles, the comparative example Wafer having a Ra equal to or higher than that of the case of using the polishing fine particles (polishing slurry) 1 or the polishing fine particles (polishing slurry) of Comparative Example 2, improving the surface roughness of the polished wafer, and having a high flatness Was obtained.

  From the above results, when the abrasive fine particles of the present invention are used as an abrasive (abrasive) of a polishing liquid (polishing slurry), polishing or grinding of a difficult-to-process substrate such as a sapphire substrate can be performed at a high rate (high polishing or grinding speed). Since it can be performed, it has been found that the processing time of a difficult-to-process substrate can be reduced and the manufacturing cost of the difficult-to-process substrate can be reduced. Further, by performing polishing or grinding of the substrate with a polishing liquid (polishing slurry) containing the polishing fine particles of the present invention, the projections on the surface of the substrate can be flattened, and the surface roughness (Ra) is improved and the flatness is improved. It has been found that a substrate having a high polishing quality can be obtained.

  The polishing fine particles of the present invention can perform polishing or grinding of a difficult-to-process substrate such as a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate at a high rate (high polishing or grinding speed), and stably perform high polishing. Since the quality can be maintained, it is possible to provide a polishing liquid (polishing slurry) capable of shortening the processing time of a difficult-to-process substrate and reducing the manufacturing cost of the difficult-to-process substrate.

Claims (13)

Having diamond particles and a carbon-containing structure derived from a fullerene derivative immobilized on the surface of the diamond particles,
In the Raman spectrum obtained by the light having an excitation wavelength of 532 nm, the maximum intensity of the peaks present in the region of 1300～1350Cm ^-1 derived from the diamond particles and ID, the maximum intensity of the peaks present in the region of 1400～1500Cm ^-1 Is I and the maximum intensity of the peak existing in the region of 1500 to 1650 cm ^-1 is IG, I / ID is 0 or more and less than 0.05, and IG / ID is 0 or more and less than 0.005. Abrasive fine particles. In a C1s photoelectron spectrum obtained by surface analysis of the carbon-containing structure using X-ray photoelectron spectroscopy, the maximum intensity within a binding energy range of 283.8 to 284.2 eV is 1 cps, and the binding energy is 284. 2. The polishing fine particles according to claim 1, wherein the ratio of 1 cps / second cps is 1.35 or more when the maximum intensity in the range of 0.8 to 285.2 eV is set to 2 cps. The ratio of the absorption peak intensity at 2800 to 3000 cm ⁻¹ in the Fourier transform infrared spectroscopy attributed to carbon-hydrogen stretching vibration is relative to the absorption peak intensity at 3000 to 3600 cm ⁻¹ assigned to oxygen-hydrogen stretching vibration. 2. The abrasive fine particles according to claim 1, wherein the abrasive fine particles have a size of 0 or more and 0.5 or less. The polishing fine particles according to claim 1, wherein the carbon-containing structure is present on a part or the whole of the surface of the diamond particles. The polishing fine particles according to claim 1, wherein the thickness of the carbon-containing structure is 1 nm or more and 100 nm or less. The fullerene derivative is a fullerene C _60, abrasive particles of claim 1. The polishing fine particles according to claim 1, wherein the average particle diameter of the polishing fine particles is 0.006 µm or more and 10.1 µm or less. The polishing fine particles according to claim 1, which is used for polishing or grinding a difficult-to-process substrate. The polishing fine particles according to claim 8, wherein the difficult-to-process substrate is a SiC substrate, a GaN substrate, a sapphire substrate, or a diamond substrate. Diamond particles, a method for producing abrasive fine particles having a carbon-containing structure derived from a fullerene derivative immobilized on the surface of the diamond particles,
Adding and mixing a fullerene derivative in a solution in which the diamond particles are dispersed, and attaching the fullerene derivative to the surface of the diamond particles;
Irradiating the diamond particles to which the fullerene derivative is attached with microwaves to transform the fullerene derivative into a carbon-containing structure, and fixing the carbon-containing structure to the diamond particles. Do
A method for producing abrasive fine particles. The method according to claim 10, wherein a main frequency of the microwave is 0.5 GHz or more and 15 GHz or less. The fullerene derivative is a fullerene C _60, A method of making an abrasive particle according to claim 10. The method according to claim 10, wherein the solution is an aqueous solution.

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