JP2003277731A - Abrasive particles and abrasives - Google Patents

Abstract

(57) [Summary] [PROBLEMS] To suppress the polishing rate for metal oxides and increase the smoothness of the polished surface without greatly changing the polishing rate for metals. SOLUTION: As the inorganic oxide particles constituting the polishing particles, particles composed of inorganic oxides such as silica, alumina, zirconia, titania and ceria, and composite inorganic oxides such as silica-alumina and silica-zirconia are preferable. It is. Since an organic functional group (R) exists on the surface of the surface-treated polishing particles, the polishing rate for a metal oxide insulating film such as silica can be suppressed, and at this time, polishing for a metal substrate such as copper can be performed. Speed does not change much.

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD The present invention relates to abrasive particles obtained by surface-treating inorganic oxide particles and an abrasive containing the abrasive particles, and particularly to abrasive particles useful in the formation of a metal wiring layer in a semiconductor integrated circuit and the like. The present invention relates to an abrasive containing the abrasive particles.

[0002]

BACKGROUND OF THE INVENTION Various integrated circuits are used in computers and various electronic devices.
With higher performance, higher density and higher performance of circuits are advancing. Conventionally, for example, in a semiconductor integrated circuit, multi-layer wiring is used to increase the degree of integration, and such multi-layer wiring is usually formed by forming a thermal oxide film as a first insulating film on a substrate such as silicon. Then, a first wiring layer made of an aluminum film or the like is formed, and an interlayer insulating film such as a silica film or a silicon nitride film is deposited on the first wiring layer by a CVD method or a plasma CVD method. Forming a silica insulating film for flattening the interlayer insulating film by the SOG method, further depositing a second insulating film on the silica insulating film as necessary, and then forming a second wiring layer. Is manufactured by. In the wiring made of the aluminum film, the wiring made of aluminum or the like may be oxidized during the sputtering when forming the multilayer wiring, and the resistance value may increase to cause a conductive failure. Further, there is a limit to forming a high-density integrated circuit because the wiring width cannot be reduced. Further, in recent years, in long-distance wiring such as clock lines and data bus lines, the wiring resistance increases as the chip size increases, and wiring delay (electrical signal propagation delay time: RC delay time = resistance x capacitance) increases. Has become. Therefore, it is necessary to replace the wiring with a material having a lower resistance.

It has been proposed to use Cu wiring instead of the conventional wiring made of Al or Al alloy. For example, after forming a wiring groove in an insulating film on a substrate in advance, electrolytic plating, C
A method of forming Cu wiring by the VD method or the like is known.
In forming a wiring pattern of copper or the like, a damascene process using a chemical mechanical polishing method (hereinafter, also referred to as CMP) is applied because processing by a dry etching process is difficult, and insulation on a substrate is applied. A wiring groove is formed in advance in the film, copper is embedded in the wiring groove by an electrolytic plating method, a CVD method, or the like, and then an upper end surface is polished by CMP and flattened to form a wiring. For example, a wiring interlayer film (insulating film) is formed on a substrate such as a silicon wafer, a groove pattern for metal wiring is formed on the wiring interlayer film (insulating film), and if necessary, a sputtering method or the like is used. TaN
A barrier metal layer such as is formed, and then copper for metal wiring is formed by the CVD method or the like. Here, when a barrier metal layer such as TaN is provided, it is possible to prevent the insulation property of the interlayer insulating film from being deteriorated due to the diffusion or erosion of copper or impurities into the interlayer insulating film, and to prevent the interlayer insulating film from being formed. And the adhesion of copper can be increased.

Then, unnecessary copper and a barrier metal (sometimes referred to as a sacrificial layer) formed outside the groove are subjected to CMP.
Then, the upper surface is planarized as much as possible, and the copper wiring / circuit pattern is formed by leaving the metal film only in the groove. In CMP, a polishing pad is generally mounted on a circular platen having a rotating mechanism, and the material to be polished is rotated while the abrasive is dropped and supplied from the upper center of the polishing pad, and the polishing pad is brought into contact with the polishing pad while applying a load. By doing so, the copper and the barrier metal in the upper portion of the coplanar surface are polished and removed. Abrasives used in CMP are usually spherical polishing particles made of metal oxides such as silica and alumina and having an average particle diameter of about 200 nm, and an oxidizer for increasing the polishing rate of wiring / circuit metals. It is composed of additives such as organic acids and solvents such as pure water.

Since there is a step (unevenness) on the surface of the material to be polished due to the wiring groove pattern formed in the underlying insulating film, the coplanar surface is polished mainly while removing the convex portion by polishing.
It is required to have a flat polished surface. However, it is difficult to stop polishing on the coplanar surface immediately after the metal portion of the convex portion is completely polished and removed, and the polishing surface of the metal portion and the newly exposed metal are stopped while actually polishing. The insulating film portion made of oxide progresses to be polished (over-polished) to a level below the coplanar surface. Therefore, the wiring resistance is increased due to the reduction of the wiring thickness, the wiring delay occurs, the integrated circuit, etc. There was a problem that the production efficiency of the. Under such circumstances, it is required to suppress the polishing rate of the insulating film portion without changing the polishing rate of the metal portion.

[0006]

It is an object of the present invention to provide a polishing particle and a polishing particle which can suppress the polishing rate for a metal oxide and can improve the smoothness of a polished surface without largely changing the polishing rate for a metal. It is intended to provide an abrasive containing the same.

[0007]

SUMMARY OF THE INVENTION The polishing particles of the present invention are characterized in that inorganic oxide particles are surface-treated with a hydrolyzable organosilicon compound represented by the following general formula. However, in the general formula, n is 1, 2 or 3, R is an unsubstituted or substituted hydrocarbon group having 1 to 10 carbon atoms, and when n is 2 or 3, they may be the same or different. May be. X: an alkoxy group having 1 to 4 carbon atoms, a silanol group, halogen, or hydrogen. R _n SiX _4-n wherein abrasive particles are in the range the average particle size of 5 to 300 nm, the hydrolyzable organosilicon compound R _n SiO
It is preferable that the content of _{(4-n) / 2} is 0.01 to 5% by weight. The abrasive of the present invention is characterized in that the polishing particles are dispersed in an aqueous dispersion medium in the range of 2 to 50% by weight.

[0008]

DETAILED DESCRIPTION OF THE INVENTION 1. First, the polishing particles of the present invention will be specifically described. Inorganic Oxide Particles The inorganic oxide particles constituting the polishing particles of the present invention are not particularly limited as long as they are particles conventionally used as polishing particles, for example, inorganic oxides such as silica, alumina, zirconia, titania and ceria. Particles composed of a complex inorganic oxide such as a substance, silica / alumina, or silica / zirconia are suitable. The shape of the inorganic oxide particles is not particularly limited,
In addition to spherical particles, rod-shaped particles, chain-shaped particles and the like, polyhedral particles can be used. In particular, spherical particles are preferable because scratches (scratches) are not generated on the polished surface. The average particle diameter of the spherical particles is generally 5 to 300 nm, especially 10 to 1
It is preferably in the range of 00 nm.

Hydrolyzable Organosilicon Compound As the surface treatment material for the polishing particles according to the present invention, a hydrolyzable organosilicon compound represented by the following general formula is used. However, in the following general formula, n: 1, 2 or 3, R: an unsubstituted or substituted hydrocarbon group having 1 to 10 carbon atoms, and when n is 2 or 3, they may be the same or different. May be. X: an alkoxy group having 1 to 4 carbon atoms, a silanol group, halogen, or hydrogen. R _n SiX _4-n Specific examples of the hydrolyzable organic group-containing silicon compound represented by the above general formula include methyltrimethoxysilane, dimethyldimethoxysilane, phenyltrimethoxysilane, diphenyldimethoxysilane, and methyltriethoxysilane. , Dimethyldiethoxysilane, phenyltriethoxysilane, diphenyldiethoxysilane, isobutyltrimethoxysilane, vinyltrimethoxysilane, vinyltriethoxysilane, vinyltris (βmethoxyethoxy) silane, 3,3,3-trifluoropropyltrimethoxy Silane, methyl-3,3,3-trifluoropropyldimethoxysilane, β- (3,4epoxycyclohexyl) ethyltrimethoxysilane, γ-glycidoxytripropyltrimethoxysilane, γ-glycidoxypropyl Tyldiethoxysilane, γ-glycidoxypropyltriethoxysilane, γ-methacryloxypropylmethyldimethoxysilane, γ-methacryloxypropyltrimethoxysilane, γ-methacryloxypropylmethyldiethoxysilane, γ-methacryloxypropyltriethoxy Silane, N-β (aminoethyl) γ-aminopropylmethyldimethoxysilane, N-β (aminoethyl) γ-aminopropyltrimethoxysilane, N-β
(Aminoethyl) γ-aminopropyltriethoxysilane, γ-aminopropyltrimethoxysilane, γ-aminopropyltriethoxysilane, N-phenyl-γ-aminopropyltrimethoxysilane, γ-mercaptopropyltrimethoxysilane, trimethylsilanol , Methyltrichlorosilane, methyldichlorosilane, dimethyldichlorosilane, trimethylchlorosilane, phenyltrichlorosilane, diphenyldichlorosilane, vinyltrichlorosilane, trimethylbromosilane, diethylsilane and the like.

Siliconization containing such hydrolyzable organic groups
The compound is R in the polishing particles._nSiO _{(4-n) / 2}As 0.
In the range of 01-5% by weight, and more preferably 0.05-5% by weight
It is preferable to contain. The content is 0.01% by weight
When it is less than 1, the amount of organic functional groups (R) on the surface of the polishing particles is small.
Therefore, it is not suitable for metal oxide insulation film and metal nitride insulation film.
It is impossible to control the polishing speed, and the wiring thickness is reduced.
Wiring resistance increases a little (sometimes called erosion)
May decrease the production efficiency of integrated circuits.
It In addition, scratches on the polished surface of metals and metal oxides
The effect of suppressing growth may not be obtained. Meanwhile, the above
Loading above 5% by weight with respect to the content
Molecular weight of water-decomposable organosilicon compounds and average of polishing particles
Although it depends on the particle size, it is almost impossible and
However, without significantly changing the polishing rate for metal,
A polishing rate suppressing effect on the insulating film, and a scraper.
The effect of suppressing the generation of
Yes.

The polishing particles of the present invention have an average particle size of 5 to 5.
It is preferably 300 nm, more preferably 10 to 100 nm. If the average particle size is less than 5 nm, the stability of the polishing particles in the polishing material may be insufficient, and the particle size may be too small to obtain a sufficient polishing rate. If the average particle size exceeds 300 nm,
Depending on the type of material to be polished (metal substrate, metal oxide insulating film substrate, etc.), scratches may be generated and sufficient smoothness may not be obtained.

Since the polishing particles of the present invention have an organic functional group (R) on the surface thereof, the polishing rate for a metal oxide insulating film such as silica can be suppressed, and at this time, a metal such as copper can be used. Since the polishing rate for the substrate does not change significantly, as a result, the above-mentioned overpolishing is suppressed, and thus the thickness of the wiring can be maintained and the wiring resistance does not increase.

Method for Producing Abrasive Particles In order to produce the abrasive particles of the present invention, it is sufficient that the surface of the inorganic oxide particles can be coated with the hydrolyzable organosilicon compound. The surface treatment method according to can be adopted. For example, a hydrolyzable organosilicon compound is added to the inorganic oxide particle dispersion liquid, and in the presence of a hydrolysis catalyst such as an acid or a base, if necessary, the inorganic oxide particles are brought into contact with the hydrolyzable organosilicon compound, It can be obtained by hydrolyzing a hydrolyzable organosilicon compound. At this time, the hydrolyzable organosilicon compound produces a silanol group by hydrolysis, and the silanol group and the OH group on the surface of the inorganic oxide particles are bonded by a hydrogen bond or the like. The mixing ratio of the inorganic oxide particles and the hydrolyzable organosilicon compound is such that polishing particles having the above-mentioned predetermined content of the hydrolyzable organosilicon compound can be obtained.

2. Next, the abrasive of the present invention will be described in detail. In the abrasive of the present invention, the aqueous dispersion medium, in addition to the aqueous dispersion medium, alcohols such as methyl alcohol, ethyl alcohol, isopropyl alcohol, and ethers,
It refers to a mixed solvent of water and a water-soluble organic solvent such as esters and ketones. In the abrasive of the present invention, when the concentration of the polishing particles is less than 2% by weight, the concentration of the polishing particles is too low to obtain a sufficient polishing rate, and the concentration of the polishing particles is 50%.
When the content exceeds the weight%, the stability of the abrasive becomes insufficient, and a dried product may be produced and adhered in the step of supplying the abrasive, which may cause scratches.

To the polishing material of the present invention, hydrogen peroxide, peracetic acid, urea peroxide or the like or a mixture thereof is added depending on the type of the material to be polished for the purpose of improving the polishing rate of metal. be able to. Further, in order to adjust the polishing rate of a plurality of materials to be polished, acids such as sulfuric acid, nitric acid, phosphoric acid, and hydrofluoric acid, or sodium salts, potassium salts, ammonium salts of these acids, and mixtures thereof are added. Can be used. As other additives, for example, imidazole, benzotriazole, benzothiazole or the like can be used in order to form a passivation layer or a dissolution suppressing layer on the surface of the material to be polished to prevent erosion of the substrate. Further, a complex-forming material such as citric acid, lactic acid, acetic acid or oxalic acid can be used to disturb the passivation layer. In order to improve the dispersibility and stability of the abrasive slurry, cationic, anionic, nonionic and amphoteric surfactants can be appropriately selected and added.
Further, in order to enhance the effect of each of the above additives, an acid or a base is added as necessary to add p of the abrasive slurry.
H may be adjusted to about 2-11, preferably 4-9, more preferably 5-8.

[0016]

According to the abrasive particles of the present invention, the surface is treated with a hydrolyzable organosilicon compound, the number of hydroxyl groups (OH groups) on the surface of the inorganic oxide particles is small, and the surface has an organic functional group. Therefore, it is possible to suppress the polishing rate for the metal oxide insulating film, the metal nitride insulating film, etc. without largely changing the polishing rate for the metal, and suppress overpolishing (erosion) of the metal oxide insulating film, etc. be able to. Therefore, the circuit resistance of the integrated circuit is not increased, scratches are not generated on the polished surface of the metal or metal oxide, and the smoothness can be improved. According to the abrasive of the present invention, in polishing in the formation of a semiconductor integrated circuit or the like, the polishing rate for a metal oxide insulating film, a metal nitride insulating film, etc. is suppressed without significantly changing the polishing rate for a metal, and overpolishing ( Erosion), which does not increase the circuit resistance of the resulting integrated circuit, and the surface after polishing is smooth,
Since the flatness is excellent, it is possible to obtain an integrated circuit that is efficiently stacked.

[0017]

Example 1 Dispersion liquid of polishing particles (A) Silica particle dispersion sol as metal oxide particles (manufactured by Catalysts & Chemicals Industry Co., Ltd .: Cataloid SI-45P, average particle diameter 45)
nm, SiO ₂ concentration 40.2% by weight) was diluted with 3020 g of ultrapure water to prepare a silica particle dispersion having an SiO ₂ concentration of 10% by weight. While stirring this, the temperature was raised to 60 ° C., and methyltrimethoxysilane (MTMS) was added to this.
A mixture of 12.6 g and 107.4 g of ethanol was added to 60
It was added in minutes and then aged for a further 60 minutes. After aging, the mixture was concentrated with an ultrafiltration membrane to obtain a dispersion liquid of polishing particles (A) having a solid content concentration of 20% by weight. At this time, the content of the hydrolyzable organosilicon compound in the polishing particles (A) is CH.
It was _1.55 % by weight as ₃ SiO _3/2 . Table 1 shows the composition and properties of the polishing particles (A).

Abrasive and polishing test (1) Abrasive Abrasive particles (A) dispersion 500 g, concentration 30% by weight
Was mixed with 333 g of hydrogen peroxide solution, 5 g of ammonium oxalate and 162 g of water to prepare an abrasive (A) having a particle concentration of 10% by weight, hydrogen peroxide of 10% by weight, and ammonium oxalate of 0.5% by weight.

(2) An insulating film made of silicon nitride (having a thickness of 0.2
Insulating film made of silica (thickness 0.4 μm)
m) is laminated, and a positive type photoresist is applied on a silicon wafer (8 inch wafer) substrate on which an insulating film (thickness 0.2 μm) made of silicon nitride is sequentially formed, and a line and space of 0.3 μm is applied. Exposure processing was performed. Then, the exposed portion was removed with a developer of tetramethylammonium hydride (TMAH). Next, a mixed gas of CF ₄ and CHF ₃ is used to form a pattern on the lower insulating film, and then the resist is removed by O ₂ plasma to obtain a width (W _C ) of 0.3 μm and a depth of 0 μm. .6
A wiring groove of μm was formed. Next, a thin layer of copper (Cu) is formed by a CVD method on the substrate in which the wiring groove is formed, and further, a film is formed by an electrolytic plating method so that the total thickness of the copper layer (sacrificial layer) on the insulating film is 0. A 2 μm copper film was formed to prepare a polishing substrate.

(3) Polishing Test Polishing substrate is polished by a polishing apparatus (Nano Factor Co., Ltd .: NF
300), the substrate load is 5 psi, the table rotation speed is 50 rpm, and the spindle speed is 60 rpm.
The polishing agent (A) was used at 60 ml / min, and polishing was performed until the sacrificial layer (thickness: 0.2 μm) on the insulating film was removed. The thickness of the insulating film portion after polishing, the thickness of the copper layer is measured, the polishing rate of the copper layer is obtained from the thickness of the copper layer, and the overpolishing (erosion, that is, the insulating portion The degree of decrease (thickness) was evaluated, and the smoothness (presence or absence of scratches) of the polished surface of the copper layer and the insulating film portion was observed, and the results are shown in Table 2.
The smoothness of the polished surface was evaluated by observing the surfaces of the copper layer and the insulating film portion after polishing with an optical microscope and the following criteria. ◯: No scratches, streaks, etc. (scratches) were observed, and the surface was smooth. Δ: Scratches and streaks (scratches) are slightly observed, but the surface is smooth. X: Many scratches, streaks, etc. (scratches) were observed, and the surface was rough. The evaluation of overpolishing was performed by measuring the decrease in the thickness of the insulating film at the beginning of formation and evaluating it according to the following criteria. ◯: Reduction in thickness is less than 10 nm. Δ: The decrease in thickness is 10 to less than 30 nm. X: The decrease in thickness is 30 nm or more.

[0021]

Example 2 Abrasive particle (B) dispersion and abrasive particles
(B ) In Example 1, methyltrimethoxysilane (MTM
S) A dispersion of polishing particles (B) having a solid content concentration of 20% by weight was obtained in the same manner as in Example 1 except that a mixed solution of 2.45 g of ethanol and 117.5 g of ethanol was added over 60 minutes. The content of the hydrolyzable organosilicon compound in the polishing particles (B) was 0.3% by weight as CH ₃ SiO _3/2 . An abrasive material (B) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (B) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0022]

Example 3 Abrasive Particle (C) Dispersion Liquid and Abrasive Particles
(C ) In Example 1, methyltrimethoxysilane (MTM
S) 6 mL of a mixture of 24.5 g and 95.5 g of ethanol
A dispersion liquid of polishing particles (C) having a solid content concentration of 20% by weight was obtained in the same manner as in Example 1 except that the addition was carried out for 0 minutes. The content of the hydrolyzable organosilicon compound in the polishing particles (C) was 3.0% by weight as CH ₃ SiO _3/2 . An abrasive (C) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (C) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.
It was shown to.

[0023]

Example 4 Abrasive Particle (D) Dispersion Liquid and Abrasive Particles
(D ) In Example 2, a mixed solution of 5.65 g of γ-glycidoxypropyltrimethoxysilane (KBM-403 manufactured by Shin-Etsu Chemical Co., Ltd.) and 114.35 g of ethanol was used as the hydrolyzable organosilicon compound. A dispersion of polishing particles (D) having a solid content concentration of 20% by weight was obtained in the same manner as in Example 2 except that the addition was performed in minutes. The content of the hydrolyzable organosilicon compound in the polishing particles (D) is C ₅ H ₁₀ O ₂ SiO.
It was 1.0% by weight as _3/2 . An abrasive (D) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (D) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0024]

Example 5 Abrasive Particle (E) Dispersion Liquid and Abrasive Particles
(E ) In the same manner as in Example 4 except that a mixed solution of 17.1 g of γ-glycidoxypropyltrimethoxysilane and 102.9 g of ethanol was added over 60 minutes, the solid content concentration was 20% by weight. A dispersion of polishing particles (E) was obtained. The content of the hydrolyzable organosilicon compound in the polishing particles (E) was 3.0% by weight as C ₅ H ₁₀ O ₂ SiO _3/2 .
Met. An abrasive (E) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (E) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0025]

Example 6 Abrasive Particle (F) Dispersion Liquid and Abrasive Particles
(F ) In Example 1, silica particles dispersed sol as an inorganic oxide particle (Cataloid SI-80 manufactured by Catalysts & Chemicals Industry Co., Ltd.)
P, average particle diameter 80 nm, SiO ₂ concentration 40.5% by weight) was used in the same manner as in Example 1 to obtain a dispersion of polishing particles (F) having a solid content concentration of 20% by weight.
The content of the hydrolyzable organosilicon compound in the polishing particles (F) was _1.48 % by weight as CH ₃ SiO _3/2 . Example 1 except that a dispersion of abrasive particles (F) was used
An abrasive (F) was prepared in the same manner as in (1), and the polishing substrate was polished in the same manner as in Example 1 using this. The results of the polishing test are shown in Table 2.

[0026]

Example 7 Abrasive Particle (G) Dispersion Liquid and Abrasive Particles
(G ) In Example 1, 1990 g of silica particle-dispersed sol (average particle size 24 nm, concentration 20% by weight) obtained by hydrolyzing tetramethoxysilane as inorganic oxide particles was diluted with pure water to obtain a solid content concentration of 10 A dispersion of polishing particles (G) having a solid content concentration of 20% by weight was obtained in the same manner as in Example 1 except that a silica particle dispersion of 1% by weight was prepared and used. The content of the hydrolyzable organosilicon compound in the polishing particles (G) was _1.55 % by weight as CH ₃ SiO _3/2 . An abrasive (G) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (G) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.
It was shown to.

[0027]

Comparative Example 1 Abrasive Particle (H) Dispersion Liquid and Abrasive Particles
(H ) Silica particle dispersed sol as an inorganic oxide particle (Catalyst Kasei Kogyo KK: Cataloid SI-45P, average particle size 45)
nm, SiO ₂ concentration 40.2% by weight) was diluted with ultrapure water to obtain a dispersion of polishing particles (H) having a solid content (SiO ₂ ) concentration of 20% by weight. An abrasive (H) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (H) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0028]

Comparative Example 2 Abrasive Particle (I) Dispersion Liquid and Abrasive Particles
(I ) Silica particle-dispersed sol as an inorganic oxide particle (Catalyst Kasei Co., Ltd .: Cataloid SI-80P, average particle diameter 80)
nm, SiO ₂ concentration 40.5% by weight) was diluted with ultrapure water to obtain a dispersion of polishing particles (I) having a solid content (SiO ₂ ) concentration of 20% by weight. Abrasive (I) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (I) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0029]

Comparative Example 3 Abrasive Particle (J) Dispersion Liquid and Abrasive Particles
(J 2 ) As the inorganic oxide particles, silica particle-dispersed sol (average particle diameter 24 nm, concentration 20% by weight) obtained by hydrolyzing tetramethoxysilane was used as it was as a dispersion liquid of polishing particles (J). An abrasive (J) was prepared in the same manner as in Example 1 except that the dispersion liquid of abrasive particles (J) was used, and this was used to polish a polishing substrate in the same manner as in Example 1. The results of the polishing test are shown in Table 2.

[0030]

[Table 1]

[0031]

[Table 2] Polishing property Polishing speed Scratch overpolishing Insulation film (I ) Copper layer (C ) ( C) / (I) Insulation film Copper layer Insulation film (Å / min) (Å / min) Example 1 120 4100 34 ○ ○ ○ Example 2 140 4100 29 ○ ○ ○ Example 3 110 4000 36 ○ ○ ○ Example 4 140 3800 27 ○ ○ ○ Example 5 140 3900 28 ○ ○ ○ Example 6 120 2800 23 ○ ○ △ Example 7 40 1100 28 ○ ○ ○ Comparative Example 1 180 4100 23 △ △ △ Comparative Example 2 160 2800 18 △ △ × Comparative Example 3 50 1100 22 △ △ △

Continued front page    (72) Inventor Akira Nakajima             13-2 Kitaminato-cho, Wakamatsu-ku, Kitakyushu, Fukuoka             Kasei Industry Co., Ltd. Wakamatsu factory (72) Inventor Toshiro Komatsu             13-2 Kitaminato-cho, Wakamatsu-ku, Kitakyushu, Fukuoka             Kasei Industry Co., Ltd. Wakamatsu factory F term (reference) 3C058 AA07 CA01 CB01 DA02 DA12

Claims (3)

[Claims] 1. Polishing particles, wherein the inorganic oxide particles are surface-treated with a hydrolyzable organosilicon compound represented by the following general formula. R _n SiX _4-n [where n is 1, 2 or 3, R is carbon number 1 to 1
0 is an unsubstituted or substituted hydrocarbon group, and when n is 2 or 3, they may be the same or different from each other. X: an alkoxy group having 1 to 4 carbon atoms, a silanol group,
Halogen or hydrogen. ] 2. The average particle diameter is in the range of 5 to 300 nm, and the hydrolyzable organosilicon compound is R _n SiO 2.
The polishing particles according to claim 1, which are contained in the range of 0.01 to 5% by weight as _{(4-n) / 2} . 3. A polishing material comprising the polishing particles according to claim 1 or 2 dispersed in an aqueous dispersion medium in a range of 2 to 50% by weight.