WO2013191139A1 - 研磨用組成物及びそれを用いた基板の製造方法 - Google Patents
研磨用組成物及びそれを用いた基板の製造方法 Download PDFInfo
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- WO2013191139A1 WO2013191139A1 PCT/JP2013/066611 JP2013066611W WO2013191139A1 WO 2013191139 A1 WO2013191139 A1 WO 2013191139A1 JP 2013066611 W JP2013066611 W JP 2013066611W WO 2013191139 A1 WO2013191139 A1 WO 2013191139A1
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- polishing composition
- polishing
- abrasive grains
- adsorbent
- surface adsorbent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09G—POLISHING COMPOSITIONS; SKI WAXES
- C09G1/00—Polishing compositions
- C09G1/02—Polishing compositions containing abrasives or grinding agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B24—GRINDING; POLISHING
- B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
- B24B37/00—Lapping machines or devices; Accessories
- B24B37/04—Lapping machines or devices; Accessories designed for working plane surfaces
- B24B37/042—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor
- B24B37/044—Lapping machines or devices; Accessories designed for working plane surfaces operating processes therefor characterised by the composition of the lapping agent
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1409—Abrasive particles per se
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1436—Composite particles, e.g. coated particles
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/14—Anti-slip materials; Abrasives
- C09K3/1454—Abrasive powders, suspensions and pastes for polishing
- C09K3/1463—Aqueous liquid suspensions
Definitions
- the present invention relates to a polishing composition used for polishing an object to be polished comprising a crystalline metal compound and a method for producing a substrate using the same.
- oxides such as aluminum oxide (for example, sapphire), silicon oxide, gallium oxide, and zirconium oxide, nitrides such as aluminum nitride, silicon nitride, and gallium nitride
- carbides such as silicon carbide are known. Since a substrate or a film formed from these materials is generally stable against chemical action such as oxidation, complexation, and etching, processing by polishing is not easy. Therefore, processing by grinding or cutting using a hard material is common. However, a surface having high smoothness could not be obtained by grinding or cutting.
- the present invention has been made by paying attention to the amount of adsorption of the surface adsorbent to the abrasive grains and finding a polishing composition capable of suppressing surface defects of the object to be polished.
- a polishing composition used for polishing a polishing object containing abrasive grains and water and made of a crystalline metal compound.
- the polishing composition further contains a surface adsorbent. The polishing composition reduces surface defects of the object to be polished compared to the case where the surface adsorbent is omitted from the polishing composition.
- the surface adsorbent is preferably at least one selected from vinyl polymers, polyalkylene oxides, and copolymers of polyalkylene oxides and alkyl groups or alkylene groups.
- the said abrasive grain and the said surface adsorbent prepared the 1st suspension containing the said abrasive grain and the said surface adsorbent as much as each content of the abrasive grain and the surface adsorbent in the said polishing composition.
- the surface adsorbent in the suspension is selected so as to satisfy the condition that 15% by mass or more of the surface adsorbent is adsorbed on the abrasive grains in the suspension.
- the surface adsorbent contains particles made of the same metal compound that constitutes the polishing object and the surface adsorbent in the same amount as each content of abrasive grains and surface adsorbent in the polishing composition.
- the amount of the surface adsorbent adsorbed on the metal compound particles in the second suspension is the amount of the surface adsorbent adsorbed on the abrasive grains in the first suspension. It is preferably selected so as to satisfy the condition that it is less than the amount.
- the abrasive is preferably at least one selected from silicon oxide, aluminum oxide, zirconium oxide, cerium oxide, and titanium oxide.
- the polishing object is preferably a single crystal substrate made of metal oxide, metal nitride, or metal carbide.
- the polishing object is preferably at least one selected from aluminum oxide, aluminum nitride, silicon oxide, silicon nitride, silicon carbide, gallium oxide, gallium nitride, and zirconium oxide.
- a method for producing a polishing substrate comprising a step of polishing a substrate made of a crystalline metal compound using the polishing composition of the above aspect.
- the polishing composition of this embodiment contains at least a surface adsorbent, abrasive grains, and water.
- the polishing object of this polishing composition is a crystalline metal compound.
- the surface of the object to be polished is preferably hydrophilic because it is difficult to adhere particles, and the object to be polished is more preferably made of a single crystal material from the viewpoint of few impurities.
- Specific examples of objects to be polished include oxides such as aluminum oxide, silicon oxide, gallium oxide, and zirconium oxide, nitrides such as aluminum nitride, silicon nitride, and gallium nitride, and ceramics such as carbides such as silicon carbide. Can be mentioned.
- the polishing composition is used for polishing an object to be polished made of a material that is stable against chemical action such as oxidation, complexation, and etching, and used for polishing aluminum oxide, particularly sapphire.
- the form of silicon oxide is not particularly limited, and may be quartz, glass or the like.
- the polishing object to which the polishing composition is applied may be used for any application, and may be, for example, an optical device material, a power device material, or a compound semiconductor.
- the form of the object to be polished is not particularly limited, and may be a substrate, a film, or other molded member.
- the abrasive grains contained in the polishing composition include, for example, those composed of silicon oxide, aluminum oxide, zirconium oxide, cerium oxide, and titanium oxide.
- aluminum oxide and silicon oxide are advantageous in that they are relatively easy to obtain and that it is easy to obtain a highly smooth and low-defect surface by polishing using a polishing composition.
- the adsorbability of the surface adsorbent to the object to be polished is preferably lower than the adsorbability of the surface adsorbent to the abrasive grains, so the abrasive grains are made of a material different from that of the object to be polished. It is preferable that
- the content of abrasive grains in the polishing composition is preferably 0.01% by mass or more, more preferably 0.1% by mass or more. As the abrasive content increases, the polishing rate of the object to be polished by the polishing composition is improved.
- the content of abrasive grains in the polishing composition is also preferably 50% by mass or less, and more preferably 40% by mass or less. As the abrasive content decreases, the manufacturing cost of the polishing composition is reduced, and it is easy to obtain a surface with less scratches by polishing using the polishing composition.
- the average primary particle diameter of the abrasive grains contained in the polishing composition is preferably 5 nm or more, more preferably 10 nm or more, and further preferably 20 nm or more. As the average primary particle diameter of the abrasive grains increases, the polishing rate of the object to be polished by the polishing composition increases.
- the average primary particle diameter of the abrasive grains contained in the polishing composition is preferably 2 ⁇ m or less, more preferably 500 nm or less, and even more preferably 200 nm or less. As the average primary particle diameter of the abrasive grains decreases, it is easy to obtain a surface with low defects and low roughness by polishing using the polishing composition.
- the value of the average primary particle diameter of an abrasive grain is computed from the specific surface area measured by BET method, for example. The measurement of the specific surface area of the abrasive grains can be performed using, for example, “Flow SorbII 2300” manufactured by Micromeritex.
- the surface adsorbent acts on the surface of the abrasive grains or the surface of the object to be polished and suppresses surface defects of the object to be polished.
- the surface adsorbent is a compound that exhibits adsorptivity to the surface of the abrasive grains or the surface of the object to be polished, and the polishing composition containing the compound is compared with the case where the same compound is omitted from the polishing composition.
- a water-soluble polymer that strongly suppresses surface defects is preferably used.
- the surface adsorbent contained in the polishing composition include, for example, vinyl polymers, polyalkylene oxides, and copolymers of polyalkylene oxides with alkyl groups or alkylene groups.
- vinyl polymers include, for example, polyvinyl alcohol, polyvinyl pyrrolidone, and n-polyvinylformamide.
- polyalkylene oxide include, for example, polyethylene glycol (PEG), polyethylene oxide (PEO), polypropylene glycol, polypropylene oxide, and copolymers thereof.
- the surface adsorbent may be a copolymer with another polymer containing the above polymer as a part of the structure, or a compound having a hydrophilic group such as a carboxylic acid group, a sulfonic acid group, or a phosphonic acid group. There may be.
- a surface adsorbent may be used individually by 1 type, and may be used in combination of 2 or more type.
- the size of the weight average molecular weight of the surface adsorbent contained in the polishing composition is such that the polishing composition containing the surface adsorbent is polished compared to the case where the surface adsorbent is omitted from the polishing composition. It is defined so as to reduce the surface defects of the object, and is appropriately selected in consideration of each kind, combination, etc. of the surface adsorbent, the abrasive grains, and the object to be polished.
- the surface adsorbent is polyethylene glycol, polyacrylic acid, polyvinyl pyrrolidone, or polyvinyl alcohol
- the abrasive is silica
- the object to be polished is alumina
- the weight average molecular weight of the agent is preferably 500 or more, and more preferably 5,000 or more.
- a protective film that suppresses the occurrence of defects is more likely to be formed on the surfaces of the abrasive grains and the object to be polished, so the number of surface defects due to polishing is greatly reduced.
- the polishing rate can be improved.
- the weight average molecular weight of the surface adsorbent contained in the polishing composition is preferably 1,000,000 or less, and more preferably 500,000 or less. As the weight average molecular weight of the surface adsorbent decreases, a protective film that suppresses the occurrence of defects is more likely to be formed on the surface of the object to be polished, so the number of surface defects resulting from polishing is greatly reduced.
- the content of the surface adsorbent in the polishing composition is preferably 0.002% by mass or more, more preferably 0.004% by mass or more, and further preferably 0.006% by mass or more. As the content of the surface adsorbent in the polishing composition increases, a protective film sufficient to suppress the occurrence of defects tends to be formed on the surface of the object to be polished. The number is greatly reduced.
- the content of the surface adsorbent in the polishing composition is preferably 0.5% by mass or less, more preferably 0.2% by mass or less, and further preferably 0.1% by mass or less. As the content of the surface adsorbent in the polishing composition decreases, the decrease in the polishing rate of the object to be polished by the protective film is more strongly suppressed.
- the surface adsorbent contained in the polishing composition contains abrasive grains or a polishing object. It is preferable to exhibit a predetermined adsorptive property to
- a first suspension containing the abrasive grains and the surface adsorbent as much as the respective contents of the abrasive grains and the surface adsorbent in the polishing composition was prepared.
- the condition that the surface adsorbent in the suspension is preferably 5% by mass or more, more preferably 15% by mass or more, and even more preferably 50% by mass or more is adsorbed on the abrasive grains in the suspension. It is desirable to be selected.
- the size of the abrasive grains used for the evaluation of the adsorptivity is not particularly limited, but is preferably an abrasive grain composed of fine particles suspendable in an aqueous solution, more preferably the same size as the abrasive grains in the polishing composition. Abrasive grains are used.
- the surface adsorbent contains second particles containing the same metal compound that constitutes the object to be polished and the surface adsorbent as much as the respective contents of the abrasive grains and the surface adsorbent in the polishing composition.
- the suspension is prepared, it is selected so as to satisfy the condition that 5% by mass or more of the surface adsorbent in the second suspension is adsorbed on the metal compound particles in the second suspension. It is preferable that More preferably, the amount of the surface adsorbent adsorbed on the metal compound particles in the second suspension is less than the amount of the surface adsorbent adsorbed on the abrasive grains in the first suspension. Is selected to satisfy the condition.
- the size of the metal compound particles used for the evaluation of the adsorptivity is not particularly limited, but is preferably a fine metal compound that can be suspended in an aqueous solution, more preferably a metal compound particle having an average primary particle size of 5 to 1000 nm. Is used.
- the adsorptivity of the surface adsorbent to the abrasive grains or metal compound particles increases, the adhesion of the abrasive grains to the polishing object is less likely to occur, and as a result, surface defects of the polishing object are further suppressed.
- the surface adsorbent may be adsorbed not only on the abrasive grains but also on the surface of the polishing object.
- the surface adsorbent adsorbs more on the abrasive grains than the metal compound particles, the surface adsorbent's protective film forming action on the object to be polished becomes weak, and as a result, polishing can be performed at a high polishing rate.
- the method of measuring the adsorptivity of the surface adsorbent contained in the polishing composition to the abrasive grains and the object to be polished is not particularly limited, but it is preferable that the conditions of both methods are the same.
- a mixed liquid (suspension) is prepared by mixing the abrasive grains and the surface adsorbent with water. You may mix
- the mixture is shaken at room temperature (24 ° C.) for a time sufficient for the abrasive grains and the surface adsorbent to adsorb, for example 1 to 24 hours, and then the abrasive grains are removed from the supernatant by a known method such as centrifugation and filtration. To separate. By measuring the amount of total organic carbon (TOC) in the remaining supernatant, the amount of the surface adsorbent remaining in the supernatant is determined. The adsorption amount of the surface adsorbent on the final abrasive grains can be determined by the ratio of the amount of the surface adsorbent remaining in the aqueous solution to the total amount of the surface adsorbent added.
- TOC total organic carbon
- the method for measuring the adsorptivity of the surface adsorbent to the object to be polished it is possible to measure under the same conditions by using particles made of the same metal compound constituting the object to be polished instead of abrasive grains. it can.
- the polishing composition of the present embodiment contains a surface adsorbent exhibiting adsorptivity to the surface of the abrasive grains or the surface of the object to be polished, and the surface adsorbent is omitted from the polishing composition. Compared to the case, surface defects of the polishing object are reduced.
- the surface adsorbent contained in the polishing composition contains abrasive grains or objects to be polished. Those having a predetermined adsorptivity as described above are selected and used.
- the surface adsorbent in the suspension is preferably selected so as to satisfy the condition that 5% by mass, 15% by mass or 50% by mass or more of the surface adsorbent is adsorbed on the abrasive grains in the suspension.
- the surface adsorbent contains second particles containing the same metal compound that constitutes the object to be polished and the surface adsorbent as much as the respective contents of the abrasive grains and the surface adsorbent in the polishing composition.
- the amount of the surface adsorbent adsorbed on the metal compound particles in the second suspension is smaller than the amount of the surface adsorbent adsorbed on the abrasive grains in the first suspension. It is more preferable that it is selected so as to satisfy the following condition. Thereby, in addition to being able to polish an object to be polished at a high polishing rate, surface defects of the object to be polished can be suppressed.
- a fine orange peel-like concave portion may be generated on the surface of the object to be polished after polishing with the polishing composition.
- the level difference on the surface of the object to be polished may not be eliminated and the defects may be further enlarged due to the adhesion of the abrasive grains to the level difference portion of the minute recess.
- the surface adsorbent adheres to the abrasive grains, thereby eliminating the level difference on the surface of the polishing object.
- the polishing composition of this embodiment is used, for example, in the production of a substrate made of a crystalline metal compound.
- the polishing pad is pressed against the surface and the substrate and the polishing pad are rotated.
- the surface of the substrate is polished by a physical action due to friction between the polishing pad and the substrate surface.
- the surface of the substrate is also polished by a physical action due to friction between the abrasive grains and the substrate surface.
- the polishing composition can suppress surface defects of the object to be polished by containing a predetermined surface adsorbent.
- the surface adsorbent in the polishing composition is at least one selected from vinyl polymers, polyalkylene oxides, and copolymers of polyalkylene oxides and alkyl groups or alkylene groups, an object to be polished Can be polished at a higher polishing rate, and surface defects of the object to be polished can be further suppressed.
- the first suspension in which the abrasive grains and the surface adsorbent in the polishing composition contain the same amount of abrasive grains and the surface adsorbent as the respective contents of the abrasive grains and the surface adsorbent in the polishing composition.
- the liquid was prepared, it was selected to satisfy the condition that 5% by mass, 15% by mass or 50% by mass or more of the surface adsorbent in the suspension was adsorbed on the abrasive grains in the suspension.
- polishing target object with a high polishing rate the surface defect of a polishing target object can be suppressed more.
- the surface adsorbent in the polishing composition is composed of the same metal compound as that constituting the object to be polished, and the surface adsorbent contains the abrasive grains and the surface adsorbent in the polishing composition.
- the second suspension containing the same amount is prepared, the amount of the surface adsorbent adsorbed on the metal compound particles in the second suspension is adsorbed on the abrasive grains in the first suspension. If selected to satisfy the condition that it is less than the amount of adsorbent, in addition to being able to polish the object to be polished at a higher polishing rate, the surface defects of the object to be polished are further suppressed. be able to.
- the surface adsorbent in the polishing composition one having a predetermined adsorptivity with respect to the abrasive grains and the object to be polished is used.
- a person skilled in the art can polish a polishing object at a high polishing rate and suppress surface defects of the polishing object from among a variety of known surface adsorbents and abrasive grains. It is possible to select the combination of the surface adsorbent and the abrasive grains, and to determine the usage amount of the surface adsorbent and the abrasive grains without performing a polishing test.
- the polishing composition of the present embodiment the effect of suppressing surface defects can be improved. Therefore, the polishing cost can be reduced by reducing the amount of abrasive grains used.
- the polishing composition may contain known additives such as antiseptics and fungicides, if necessary.
- the polishing composition may be in a concentrated state at the time of manufacture and sale. That is, the polishing composition may be manufactured and sold in the form of a stock solution of the polishing composition.
- the polishing composition may be prepared by diluting a stock solution of the polishing composition with water.
- each component contained in the polishing composition may be filtered by a filter immediately before production. Further, the polishing composition may be used after being filtered through a filter immediately before use. By performing the filtration treatment, coarse foreign matters in the polishing composition are removed, and the quality is improved.
- the polishing pad used in the polishing method using the polishing composition is not particularly limited. For example, you may use a nonwoven fabric type and a suede type.
- the used polishing composition used for polishing the substrate may be collected and reused (circulated). More specifically, the used polishing composition discharged from the polishing apparatus may be once collected in a tank and supplied from the tank to the polishing apparatus again. In this case, since it is less necessary to treat the used polishing composition as a waste liquid, it is possible to reduce the environmental load. Moreover, the manufacturing cost of a board
- substrate can also be reduced by reducing the usage-amount of polishing composition.
- polishing composition When the polishing composition is recycled, replenishment of the reduced amount of at least one of the components such as the surface adsorbent in the polishing composition consumed or lost by being used for polishing the substrate. Preferably it is done.
- the abrasive grains in the polishing composition may be spherical or non-spherical.
- the non-spherical shape include a so-called saddle shape having a constriction at the center, a so-called confetti shape having a plurality of protrusions on the surface, and a rugby ball shape.
- a method for producing a polishing composition used for polishing a polishing object comprising a crystalline metal compound comprising: Selecting abrasive grains and surface adsorbent; Mixing the selected abrasive grains and surface adsorbent with water to obtain a polishing composition containing abrasive grains, surface adsorbent and water,
- the step of selecting the abrasive and the surface adsorbent includes When the first suspension containing the abrasive grains and the surface adsorbent in the same amount as the abrasive grains and the surface adsorbent in the polishing composition was prepared, the surface in the suspension Satisfying the condition that 15% by mass or more of the adsorbent is adsorbed on the abrasive grains in the suspension, and A second suspension containing the particles of the same metal compound that constitutes the polishing object and the surface adsorbent as much as the respective contents of the abrasive grains and the surface adsorbent in the
- a method for reducing the occurrence of orange-peeled microrecesses on the surface of a polishing object made of a crystalline metal compound comprising a surface adsorbent, abrasive grains, and water
- a step of polishing the polishing object using a polishing composition The abrasive grains and the surface adsorbent are: When the first suspension containing the abrasive grains and the surface adsorbent in the same amount as the abrasive grains and the surface adsorbent in the polishing composition was prepared, the surface in the suspension Satisfying the condition that 15% by mass or more of the adsorbent is adsorbed on the abrasive grains in the suspension, and A second suspension containing the particles of the same metal compound that constitutes the polishing object and the surface adsorbent as much as the respective contents of the abrasive grains and the surface adsorbent in the polishing composition.
- polishing composition Colloidal silica sol containing colloidal silica having an average primary particle size of 80 nm was diluted with water, and various surface adsorbents were added thereto. Then, the polishing compositions of Examples 1 to 6 and Comparative Example 1 were prepared by adjusting the pH value to 7 using nitric acid or potassium hydroxide (pH adjuster). The type and weight average molecular weight of the surface adsorbent contained in each polishing composition are as shown in the “surface adsorbent” column of Table 1. All of the polishing compositions of Examples 1 to 6 have a colloidal silica content of 5 mass% and a surface adsorbent content of 0.032 mass%.
- a control polishing composition was prepared by diluting a colloidal silica sol containing colloidal silica having an average primary particle size of 80 nm with water and adjusting the pH value to 7 using a pH adjuster.
- This control polishing composition has a colloidal silica content of 5 mass% and does not contain a surface adsorbent.
- a first suspension was prepared. Specifically, first, 1.6% by mass of the same surface adsorbent contained in each of the polishing compositions of Examples 1 to 6 and Comparative Example 1 was contained, and the pH was adjusted to 7 using nitric acid or potassium hydroxide. An adjusted aqueous solution was prepared. Then, 10 g of the aqueous solution and 2.5 g of silica having an average primary particle diameter of 80 nm were mixed with 37.5 g of water to prepare a target suspension.
- the contents of silica and surface adsorbent in each suspension are 5% by mass and 0.032% by mass, respectively, as in the polishing compositions of Examples 1 to 6 and Comparative Example 1.
- the first suspension was shaken at room temperature (24 ° C.) for 20 hours, and then the silica in the suspension was precipitated by centrifugation at 26000 rpm for 60 minutes to obtain a supernatant.
- the total organic carbon (TOC) amount in the obtained supernatant was measured using a TOC measuring device (Shimadzu Corporation: TOC-5000A), and the amount of the surface adsorbent remaining in the supernatant was determined. .
- TOC total organic carbon
- a second suspension was prepared.
- the second suspension was prepared in the same procedure as the first suspension except that 2.5 g of alumina having an average primary particle size of 400 nm was used instead of 2.5 g of silica.
- it remains in the supernatant liquid with respect to the total addition amount of the surface adsorbent in the same procedure as the amount of adsorption of the surface adsorbent on the silica except that the rotation speed at the time of centrifugation is changed from 26000 rpm to 3000 rpm. From the ratio of the amount of the surface adsorbent, the final adsorption amount of the surface adsorbent on alumina was determined. The results are shown in Table 1 and FIG.
- the surface (C-plane ( ⁇ 0001>)) of the sapphire substrate was polished using the polishing compositions of Examples 1 to 6, Comparative Example 1 and Control under the following conditions. 52 mm (about 2 inches) of the same type.
- the number (/ mm 2 ) of orange peels generated on the sapphire substrate after polishing with each polishing composition was determined using a differential interference microscope. Further, the mass of the sapphire substrate before and after polishing was measured, the polishing rate was measured from the difference in mass before and after polishing, and the ratio when the polishing rate in the case of the control polishing composition was set to 1 was determined. The results are shown in Table 1 and FIG.
- Polishing machine Lens polishing machine manufactured by Udagawa Seiko Co., Ltd.
- Polishing pad Non-woven pad SUBA800 manufactured by Nitta Haas (no groove) Polishing load: 300 g / cm 2 (29.4 kPa)
- Bottom plate rotation speed 130rpm
- Polishing composition supply rate 20 mL / min (flowing) Polishing time: 10 minutes As shown in Table 1 and FIG.
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Abstract
Description
砥粒及び表面吸着剤を選択する工程と、
その選択した砥粒及び表面吸着剤を水に混合して、砥粒、表面吸着剤及び水を含有する研磨用組成物を得る工程とを含み、
前記砥粒及び表面吸着剤を選択する工程は、
前記砥粒及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第1の懸濁液を調製したときに、前記懸濁液中の表面吸着剤の15質量%以上が前記懸濁液中の砥粒に吸着するという条件を満たし、且つ、
前記研磨対象物を構成するのと同じ金属化合物からなる粒子及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第2の懸濁液を調製したときに、前記第2の懸濁液中で金属化合物粒子に吸着する表面吸着剤の量が前記第1の懸濁液中で砥粒に吸着する表面吸着剤の量よりも少ないという条件を満たすように行われる、方法。
前記砥粒及び前記表面吸着剤は、
前記砥粒及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第1の懸濁液を調製したときに、前記懸濁液中の表面吸着剤の15質量%以上が前記懸濁液中の砥粒に吸着するという条件を満たし、且つ、
前記研磨対象物を構成するのと同じ金属化合物からなる粒子及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第2の懸濁液を調製したときに、前記第2の懸濁液中で金属化合物粒子に吸着する表面吸着剤の量が前記第1の懸濁液中で砥粒に吸着する表面吸着剤の量よりも少ないという条件を満たすように選択されたものである、方法。
平均一次粒子径が80nmのコロイダルシリカを含んだコロイダルシリカゾルを水で希釈し、それに各種の表面吸着剤を添加した。そして、pHの値を硝酸又は水酸化カリウム(pH調整剤)を用いて7に調整することにより、実施例1~6及び比較例1の研磨用組成物を調製した。各研磨用組成物中に含まれる表面吸着剤の種類及び重量平均分子量は、表1の“表面吸着剤”欄に示すとおりである。実施例1~6の研磨用組成物はいずれも、コロイダルシリカの含有量が5質量%、表面吸着剤の含有量が0.032質量%である。
砥粒を構成する材料の一例であるシリカ(SiO2)に対する表面吸着剤の吸着性について試験するために、第1の懸濁液を調製した。具体的にはまず、実施例1~6及び比較例1の各研磨用組成物中に含まれるのと同じ表面吸着剤を1.6質量%含有し、硝酸又は水酸化カリウムを用いてpH7に調整された水溶液を用意した。そして、その水溶液10gと平均一次粒子径が80nmのシリカ2.5gとを、37.5gの水に混合することにより、目的の懸濁液を調製した。各懸濁液中のシリカ及び表面吸着剤の含有量は、実施例1~6及び比較例1の研磨用組成物と同じく、それぞれ5質量%及び0.032質量%である。第1の懸濁液を室温(24℃)で20時間振とう後、26000rpmで60分間の遠心分離により、懸濁液中のシリカを沈殿させて上澄み液を得た。次に、得られた上澄み液中の全有機炭素(TOC)量を、TOC測定器(島津製作所:TOC-5000A)を用いて測定し、上澄み液中に残存する表面吸着剤の量を求めた。表面吸着剤の全添加量に対する上澄み液中に残存する表面吸着剤の量の比率から、最終的なシリカへの表面吸着剤の吸着量を求めた。結果を表1及び図1に示す。
研磨対象物を構成する材料の一例であるアルミナ(Al2O3)に対する表面吸着剤の吸着性について試験するために、第2の懸濁液を調製した。第2の懸濁液の調整は、シリカ2.5gの代わりに平均一次粒子径が400nmのアルミナ2.5gを使用した以外は第1の懸濁液と同様の手順で行った。また、遠心分離の際の回転速度を26000rpmから3000rpmに変更した以外はシリカへの表面吸着剤の吸着量を求めたのと同じ手順で、表面吸着剤の全添加量に対する上澄み液中に残存する表面吸着剤の量の比率から、最終的なアルミナへの表面吸着剤の吸着量を求めた。結果を表1及び図1に示す。
実施例1~6、比較例1及びコントロールの各研磨用組成物を用いて、下記の条件でサファイア基板の表面(C面(<0001>)を研磨した。使用したサファイア基板はいずれも、直径52mm(約2インチ)の同種のものである。
研磨機:宇田川鐵工株式会社製のレンズ研磨機
研磨パッド:ニッタ・ハース社製の不織布パッドSUBA800(溝なし)
研磨荷重:300g/cm2(29.4kPa)
底盤回転数:130rpm
研磨用組成物の供給速度:20mL/分(かけ流し)
研磨時間:10分
表1及び図2に示されるように、表面吸着剤がシリカ又はアルミナに対する吸着性を示す場合(具体的には、表面吸着剤の全添加量の5質量%以上がシリカ又はアルミナに吸着する場合)、サファイア基板の表面欠陥を抑制することができることが確認された。また、表面吸着剤の全添加量の15質量%以上がシリカに吸着する場合には、サファイア基板を高い研磨速度で研磨することができるのに加えて、サファイア基板の表面欠陥を抑制することができることが確認された。さらに、表面吸着剤がアルミナよりもシリカに多く吸着する場合には、サファイア基板をより高い研磨速度で研磨することができる傾向にあることが確認された。
Claims (8)
- 結晶性の金属化合物からなる研磨対象物を研磨する用途で使用される研磨用組成物であって、前記研磨用組成物は砥粒及び水を含有し、
前記研磨用組成物はさらに表面吸着剤を含有し、前記研磨用組成物は、前記研磨用組成物から表面吸着剤を省いた場合に比べて、研磨対象物の表面欠陥を低減することを特徴とする研磨用組成物。 - 前記表面吸着剤は、ビニル系ポリマー、ポリアルキレンオキサイド、及びポリアルキレンオキサイドとアルキル基又はアルキレン基との共重合体から選ばれる少なくとも一種であることを特徴とする請求項1に記載の研磨用組成物。
- 前記砥粒及び前記表面吸着剤は、
前記砥粒及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第1の懸濁液を調製したときに、前記懸濁液中の表面吸着剤の15質量%以上が前記懸濁液中の砥粒に吸着する
という条件を満たすように選択されたものであることを特徴とする請求項1又は請求項2に記載の研磨用組成物。 - 前記表面吸着剤は、
前記研磨対象物を構成するのと同じ金属化合物からなる粒子及び前記表面吸着剤を前記研磨用組成物中の砥粒及び表面吸着剤の各含有量と同じだけ含有する第2の懸濁液を調製したときに、前記第2の懸濁液中で金属化合物粒子に吸着する表面吸着剤の量が前記第1の懸濁液中で砥粒に吸着する表面吸着剤の量よりも少ない
という条件を満たすように選択されたものであることを特徴とする請求項1~3のいずれか1項に記載の研磨用組成物。 - 前記砥粒は、酸化ケイ素、酸化アルミニウム、酸化ジルコニウム、酸化セリウム、及び酸化チタニウムから選ばれる少なくとも一種であることを特徴とする請求項1~4のいずれか1項に記載の研磨用組成物。
- 前記研磨対象物は、金属酸化物、金属窒化物又は金属炭化物からなる単結晶基板であることを特徴とする請求項1~5のいずれか1項に記載の研磨用組成物。
- 前記研磨対象物は、酸化アルミニウム、窒化アルミニウム、酸化ケイ素、窒化ケイ素、炭化ケイ素、酸化ガリウム、窒化ガリウム、及び酸化ジルコニウムから選ばれる少なくとも一種であることを特徴とする請求項1~6のいずれか1項に記載の研磨用組成物。
- 請求項1~7のいずれか一項に記載の研磨用組成物を用いて、結晶性の金属化合物からなる基板を研磨する工程を含むことを特徴とする研磨基板の製造方法。
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