WO2016043089A1 - Composition d'agent de polissage pour substrat en saphir - Google Patents

Composition d'agent de polissage pour substrat en saphir Download PDF

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Publication number
WO2016043089A1
WO2016043089A1 PCT/JP2015/075424 JP2015075424W WO2016043089A1 WO 2016043089 A1 WO2016043089 A1 WO 2016043089A1 JP 2015075424 W JP2015075424 W JP 2015075424W WO 2016043089 A1 WO2016043089 A1 WO 2016043089A1
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WIPO (PCT)
Prior art keywords
sapphire substrate
polishing
composition
abrasive
mass
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PCT/JP2015/075424
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English (en)
Japanese (ja)
Inventor
良延 山口
内藤　健治
堀本　真樹
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山口精研工業株式会社
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Priority to JP2016548844A priority Critical patent/JPWO2016043089A1/ja
Publication of WO2016043089A1 publication Critical patent/WO2016043089A1/fr

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Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24B—MACHINES, DEVICES, OR PROCESSES FOR GRINDING OR POLISHING; DRESSING OR CONDITIONING OF ABRADING SURFACES; FEEDING OF GRINDING, POLISHING, OR LAPPING AGENTS
    • B24B37/00—Lapping machines or devices; Accessories
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
    • H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
    • H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
    • H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
    • H01L21/304—Mechanical treatment, e.g. grinding, polishing, cutting

Definitions

  • the present invention relates to an abrasive composition, particularly an abrasive composition for sapphire.
  • a hard and brittle material includes glass, ceramics, stone, semiconductor crystal material, and the like.
  • What is called a hard and brittle material is a material to be polished that is difficult to process, slows the polishing rate, requires a lot of processing time, and requires a high-quality polished surface with high flatness with very few scratches and defects.
  • a typical example of such a material to be polished is a sapphire substrate.
  • Sapphire substrates are frequently used in applications such as LED element substrates, and their production volume has increased in recent years. For example, the LED is obtained by growing a GaN film on a sapphire substrate by CVD coating. Sapphire is also used in the cover glass of smartphones and tablets.
  • sapphire is a chemically stable and extremely hard material having a Mohs hardness of 9
  • processing such as cutting, lapping and polishing is extremely difficult, and processing requires a very long time.
  • Various attempts have been made to reduce the processing time and reduce the cost as much as possible.
  • a sapphire wafer cut from a sapphire ingot is subjected to a lapping process in which diamond abrasive grains harder than sapphire are changed in a multi-stage from large abrasive grains to small abrasive grains, followed by a silica-based abrasive, especially colloidal silica-based
  • a sapphire substrate has been produced by final polishing in a polishing process using an abrasive.
  • there is a problem that production cost increases because an expensive abrasive such as diamond is used and processing time becomes long in a plurality of processing steps.
  • an abrasive composition for achieving both a high polishing rate and a reduction in scratches and defects and an improvement in flatness is disclosed.
  • Patent Document 1 discloses an abrasive for sapphire having a basic pH containing a salt compound in an aqueous medium in which alumina particles, colloidal silica and the like are suspended.
  • the salt compound is an alkali metal or alkaline earth metal salt of an acid
  • the acid here is hydrochloric acid, hydrobromic acid, hydroiodic acid, sulfuric acid, nitric acid, ascorbic acid, oxalic acid or picoline. There is a description that it is an acid.
  • Patent Document 1 does not disclose the use of alkali metal salts or alkaline earth metal salts of aluminum, silicon or boron oxoacids.
  • Patent Document 2 discloses an abrasive composition used for polishing an alumina substrate or the like, which contains colloidal silica and composite abrasive grains such as aluminum oxide. However, Patent Document 2 does not disclose the use of alkali metal salts or alkaline earth metal salts of aluminum, silicon or boron oxoacids.
  • Patent Document 3 discloses an abrasive composition used for polishing an aluminum-containing ceramic substrate, which contains an abrasive containing alumina particles and an additive containing a phosphorus compound, and has a pH of about 8 or higher. However, Patent Document 3 does not disclose the use of alkali metal salts or alkaline earth metal salts of aluminum, silicon or boron oxoacids.
  • Patent Document 4 discloses a sapphire polishing slurry containing alumina abrasive grains characterized by having a pH in the range of 10.0 to 14.0. However, Patent Document 4 does not disclose the use of alkali metal salts or alkaline earth metal salts of aluminum, silicon or boron oxoacids.
  • Patent Document 5 as an abrasive composition for hard and brittle materials having a Vickers hardness of 1500 Hv or more, an abrasive composition containing aluminum oxide abrasive grains having a pH of 8.5 or more and a surface area of 20 m 2 / g or less. Things are disclosed. However, Patent Document 5 does not disclose the use of alkali metal salts or alkaline earth metal salts of aluminum, silicon or boron oxoacids.
  • Patent Document 1 in which colloidal silica is used for abrasive grains, a satisfactory polished surface can be obtained, but a sufficient polishing rate cannot be obtained.
  • Patent Documents 2 to 5 since alumina, which is relatively hard particles, is used for the abrasive grains, the polishing rate is improved, but it cannot be said that a sufficient polishing rate is obtained. In addition, a highly accurate polished surface is not obtained after polishing.
  • the present invention has been intensively studied in view of such problems, and is a polishing composition for a sapphire substrate capable of obtaining a highly accurate polished surface with high scratching speed, low scratches, low surface roughness, and the like. Is to provide.
  • the present invention also provides an abrasive composition that can be used not only for sapphire substrates but also for hard and brittle materials such as hard glass substrates, quartz substrates, silicon and semiconductor substrates having the same problems as described above.
  • the present inventor is an abrasive composition for a sapphire substrate containing inorganic abrasive particles, a polishing accelerator, and water, wherein the inorganic abrasive particles are alumina particles, and the polishing accelerator is oxo
  • An abrasive composition for a sapphire substrate containing inorganic abrasive particles, a polishing accelerator, and water,
  • the inorganic abrasive particles are alumina particles
  • the polishing accelerator is an oxoacid salt
  • pH is 9.0-13.0
  • the oxo acid salt is an alkali metal salt or alkaline earth metal salt of aluminum, silicon or boron oxo acid
  • An abrasive composition for a sapphire substrate characterized in that.
  • the content of the oxoacid salt is any one of the above [1] to [3], wherein the content of the oxoacid salt is 0.01 to 5% by mass with respect to the mass of the sapphire substrate polishing composition.
  • the above-mentioned dispersant is at least one selected from the group consisting of polycarboxylic acids (salts), copolymers containing repeating units of polycarboxylic acids (salts), and condensed phosphates.
  • abrasive composition for sapphire substrates is at least one compound selected from the group consisting of alumina sol and celluloses.
  • a method for polishing a sapphire substrate comprising polishing using the abrasive composition for sapphire substrate according to any one of [1] to [16]
  • a method for producing a sapphire substrate comprising a step of polishing using the sapphire substrate abrasive composition according to any one of [1] to [16].
  • the abrasive composition of the present invention can polish a hard and brittle material such as a sapphire substrate at high speed, and can finish the polished surface to a high quality polished surface with high flatness and few scratches and defects.
  • the abrasive composition of the present invention is particularly suitable for polishing sapphire substrates.
  • the abrasive composition of the present invention can reduce the polishing time and polish a sapphire substrate or the like at a low cost.
  • the abrasive composition for a sapphire substrate of the present invention contains inorganic abrasive particles, a polishing accelerator, and water, the inorganic abrasive particles are alumina particles, and the polishing accelerator is an oxoacid salt.
  • the pH of the abrasive composition for sapphire substrate is 9.0 to 13.0, and the oxo acid salt is an alkali metal salt or alkaline earth metal salt of aluminum, silicon or boron oxo acid.
  • the abrasive composition of the present invention contains inorganic abrasive particles, and the inorganic abrasive particles are alumina particles. If necessary, silicon oxide, zircon, zirconium oxide, cerium oxide, silicon nitride, silicon carbide, etc. may be added to the inorganic abrasive particles.
  • gibbsite Al 2 O 3 ⁇ 3H 2 O boehmite Al 2 O 3 ⁇ H 2 O
  • pseudoboehmite Al 2 O 3 ⁇ nH 2 O (n 1 ⁇ 2)
  • ammonium Examples thereof include aluminum salts such as alum AlNH 4 (SO 4 ) 2 ⁇ 12H 2 O and ammonium dosonite NH 4 AlCO 3 (OH) 2 .
  • These alumina raw materials are prepared, for example, by the following method.
  • ammonium alum is obtained by cooling an aqueous solution of ammonium sulfate and aluminum sulfate and precipitating from the solution.
  • Ammonium dosonite is obtained by reacting ammonium alum and ammonium carbonate.
  • Alumina can be obtained by firing or pyrolyzing these alumina raw materials.
  • Alumina particles can be obtained by pulverizing and classifying the obtained alumina.
  • Alumina particles have various crystal forms such as ⁇ -alumina, ⁇ -alumina, ⁇ -alumina, and ⁇ -alumina, and any crystal form can be used.
  • alumina particles made from boehmite or pseudo-boehmite can be used to obtain round and polycrystalline alumina particles, which makes it easier to obtain relatively high-purity alumina particles. Further, when preparing the particle size, it is easy to obtain fine particles with few coarse particles, narrow particle size distribution, and few corners. Since alumina particles having such characteristics are used, when alumina particles made from boehmite or pseudoboehmite are used in the abrasive composition for sapphire substrates of the present invention, scratches on the substrate are reduced and a high polishing rate is obtained. Can do.
  • the D50 value (median diameter) of the inorganic abrasive particles of the present invention is preferably 0.01 to 1.00 ⁇ m.
  • D50 is smaller than 0.01 ⁇ m, it is difficult to obtain a sufficient polishing rate.
  • D50 is larger than 1.00 ⁇ m, surface quality deterioration of the polished surface such as generation of scratches and latent scratches, deterioration of surface roughness, and deterioration of flatness is caused. You may be invited.
  • the dispersion stability (how long a dispersed state can be maintained in an aqueous medium without settling of particles) may be deteriorated.
  • D50 is more preferably 0.10 to 0.90 ⁇ m, still more preferably 0.20 to 0.70 ⁇ m.
  • D50 can be measured using a laser diffraction particle size distribution analyzer (for example, SALD2200, manufactured by Shimadzu Corporation).
  • SALD2200 laser diffraction particle size distribution analyzer
  • D50 is the particle size distribution measured on the basis of volume based on the laser diffraction method. When the measured particle diameters are integrated in order of increasing particle diameter starting from the smallest particle diameter, It is the particle diameter that occupies 50% of the volume of the particles. For example, D50 of 0.45 ⁇ m means that the total volume of particles having a particle diameter of 0.45 ⁇ m or less occupies 50% of the total volume of all target particles.
  • the specific surface area of the inorganic abrasive particles of the present invention is preferably 0.1 to 15 m 2 / g.
  • the specific surface area of the alumina abrasive grains gradually becomes a small value by firing or pyrolysis of the alumina raw material, and can be adjusted according to the firing and pyrolysis conditions.
  • the specific surface area is smaller than 0.1 m 2 / g, the surface roughness increases and scratches may increase.
  • the specific surface area is larger than 15 m 2 / g, it is difficult to obtain a sufficient polishing rate.
  • the specific surface area is more preferably 1 to 14 m 2 / g.
  • the specific surface area can be measured as a BET value using a flow-type specific surface area automatic measuring device (for example, Flowsorb II manufactured by Shimadzu Corporation).
  • the BET value is a specific surface area determined by the BET method (gas adsorption method).
  • the crystal form of the alumina particles of the present invention is preferably ⁇ -alumina.
  • the alumina raw material When the alumina raw material is fired or pyrolyzed, it undergoes a crystal phase transition to an ⁇ crystal, which is a high-temperature stable phase, through crystal phases such as ⁇ crystal, ⁇ crystal, and ⁇ crystal. Since the crystal phase increases in hardness and the size of crystal grains grows as firing and pyrolysis occur, the crystal phase can be adjusted according to the firing and pyrolysis conditions.
  • the alumina raw material can be crystallized to ⁇ crystal by subjecting the alumina raw material to firing or thermal decomposition at a temperature of 1000 ° C. or higher. Since ⁇ -alumina is a crystal form having sufficient hardness, a high polishing rate can be obtained when ⁇ -alumina particles are used in the abrasive composition of the present invention.
  • the content of the inorganic abrasive particles of the present invention is preferably 5 to 50% by mass with respect to the mass of the abrasive composition for a sapphire substrate. If the content is less than 5% by mass, it is difficult to obtain a sufficient polishing rate. Even if the content is more than 50% by mass, no further improvement in the polishing rate is recognized and it is not economical. Dispersibility deteriorates and the viscosity of the abrasive composition increases, so that the polishing rate may decrease, and the liquid feeding resistance may increase when the abrasive composition is circulated and cause problems. is there.
  • the content of the inorganic abrasive particles is more preferably 5 to 20% by mass, and further preferably 8 to 15% by mass with respect to the mass of the abrasive composition for sapphire substrate.
  • the pH of the abrasive composition of the present invention is 9.0 to 13.0.
  • the above pH is suitable for polishing the sapphire substrate for the following reasons.
  • Sapphire is single crystal alumina, but it is known that the surface of sapphire acts as a solid acid in water. Therefore, when frictional heat is generated locally during polishing, it is considered that sapphire is alkaline liquid and the surface dissolution reaction is likely to occur due to frictional heat. It is considered that polishing is started by this dissolution reaction.
  • the pH is less than 9, the dissolution reaction does not start and the polishing rate is remarkably reduced. Even if the value exceeds 13.0, no further improvement in the polishing rate is recognized, and it is dangerous during handling.
  • the pH is more preferably 10.0 to 13.0.
  • the polishing accelerator accelerates the reaction on the surface of the sapphire substrate at a pH of 9.0 to 13.0 of the polishing composition and provides a high polishing rate.
  • an alkali metal salt or alkaline earth metal salt of aluminum, silicon or boron oxo acid is used as a polishing accelerator.
  • the abrasive composition of the present invention may optionally use an organic carboxylic acid chelating compound or an organic phosphonic acid chelating compound as a polishing accelerator.
  • the polishing accelerator referred to in the present invention is considered to have an action of promoting removal of the deteriorated layer due to dissolution generated on the surface of the sapphire substrate by the abrasive composition having a pH of 9.0 to 13.0.
  • the oxo acid of the oxo acid salt used in the present invention is preferably an oxo acid of one or more elements selected from the group consisting of aluminum, silicon and boron.
  • These oxo acid salts include aluminates, silicates, aluminosilicates, and borates. Among these, use of aluminate is preferable.
  • the salt of the oxo acid salt used in the present invention is preferably one or more salts selected from the group consisting of alkali metal salts and alkaline earth metal salts.
  • These oxo acid salts include sodium salts, potassium salts, lithium salts, calcium salts and the like. Of these, the use of sodium salt or potassium salt is preferred.
  • the oxoacid salt used in the present invention preferably contains sodium aluminate or potassium aluminate, and most preferably contains sodium aluminate.
  • Oxo acid salts are known and are readily available in the market or can be prepared.
  • the content of the oxoacid salt is preferably in the range of 0.01 to 5% by mass with respect to the mass of the abrasive composition for sapphire substrate. If the amount is less than 0.01% by mass, the effect of promoting the polishing rate is not sufficient, and if the amount exceeds 5% by mass, no further improvement in the polishing rate is recognized and it is not economical, but the dispersibility starts to deteriorate. Sometimes.
  • the content of the oxoacid salt is more preferably in the range of 0.01 to 2% by mass, and still more preferably in the range of 0.1 to 1.5% by mass with respect to the mass of the abrasive composition for sapphire substrate.
  • a chelating compound may optionally be used in combination as a polishing accelerator.
  • the chelating compound is preferably an organic carboxylic acid chelating compound or an organic phosphonic acid chelating compound. From the viewpoint of setting the pH of the abrasive composition to 9.0 to 13.0, the organic phosphonic acid chelating compound and the organic carboxylic acid chelating compound form salts with alkali metals, ammonia, amines, and the like. It is preferable.
  • These salts are produced in the abrasive composition by adding an organic phosphonic acid chelating compound or organic carboxylic acid chelating compound and an alkali metal hydroxide, ammonia or amine, respectively, to the abrasive composition.
  • organic phosphonic acid-based chelating compound include hydroxyethylidene diphosphonic acid (HEDP), nitrilotrismethylene phosphonic acid (NTMP), and their sodium, potassium, ammonium, and amine salts.
  • organic carboxylic acid chelating compounds include ethylenediaminetetraacetic acid (EDTA), nitrilotriacetic acid (NTA), diethylenetriaminepentaacetic acid (DTPA), hydroxyethylethylenediaminetetraacetic acid (HEDTA), triethylenetetraaminehexaacetic acid (TTHA), hydroxy Ethyliminodiacetic acid (HIDA), dihydroxyethylglycine (DHEG), dicarboxymethylglutamic acid (GMGA), ethylenediamine-N, N ′′ -disuccinic acid (EDDS) and their sodium, potassium, ammonium and amine salts Etc.
  • EDTA ethylenediaminetetraacetic acid
  • NTA nitrilotriacetic acid
  • DTPA diethylenetriaminepentaacetic acid
  • HEDTA hydroxyethylethylenediaminetetraacetic acid
  • TTHA triethylenetetraaminehexaacetic acid
  • the above compounds may be used alone or in combination of two or more.
  • Preferred chelating compounds include ethylenediaminetetraacetic acid-tetrapotassium salt, hydroxyethylethylenediaminetetraacetic acid-trisodium salt, hydroxyethylidene diphosphonic acid-tetrasodium salt, nitrilotrismethylenephosphonic acid-pentasodium salt, and the like. Chelating compounds are known and are readily available on the market or can be prepared.
  • the content of the chelating compound is preferably in the range of 0.01 to 5% by mass with respect to the mass of the abrasive composition for sapphire substrate. If the amount is less than 0.01% by mass, the effect of promoting the polishing rate is not sufficient, and if it exceeds 5% by mass, the dispersibility may begin to deteriorate.
  • the content of the chelating compound is more preferably in the range of 0.01 to 2% by mass, and still more preferably 0.1 to 1% by mass with respect to the mass of the sapphire substrate polishing composition.
  • the agglomeration of inorganic abrasive particles in the abrasive composition may cause a decrease in polishing surface quality and a reduction in polishing rate, such as generation of scratches and deterioration in surface roughness.
  • a dispersant may be used in combination for the purpose of improving the dispersion state of the inorganic abrasive particles and improving the above problems.
  • the dispersant include a polymer type dispersant, a surfactant type dispersant, an inorganic type dispersant, and the like.
  • the polymeric dispersant include polycarboxylic acids (salts), copolymers containing polycarboxylic acid (salt) repeating units, and inorganic dispersants include condensed phosphates.
  • polycarboxylic acid polyacrylic acid, polymethacrylic acid, polyacrylic acid alkali metal salt, polymethacrylic acid alkali metal salt, polyacrylic acid ammonium salt, polymethacrylic acid ammonium salt, polyacrylic acid amine
  • examples thereof include salts and polymethacrylic acid amine salts.
  • the copolymer containing a repeating unit of polycarboxylic acid (salt) include a copolymer of polyacrylic acid and a structural unit containing a sulfonic acid group, a copolymer of polyacrylic acid and a polyacrylate ester, and the like. It is done.
  • the condensed phosphate include sodium hexametaphosphate, sodium pyrophosphate, potassium pyrophosphate, sodium tripolyphosphate, sodium acid metaphosphate, and sodium acid pyrophosphate.
  • the content of the dispersing agent is preferably in the range of 0.005 to 0.5 mass% with respect to the mass of the abrasive composition for sapphire substrate. If it is less than 0.005% by mass, the effect of improving the dispersion state of the inorganic abrasive particles is not sufficient, and if it exceeds 0.5% by mass, the effect of improving the dispersion state of the inorganic abrasive particles reaches its peak and is economical. Not.
  • the content of the dispersant is more preferably 0.01 to 0.5% by mass, still more preferably 0.02 to 0.3% by mass, with respect to the mass of the sapphire substrate polishing composition. Most preferably, it is 0.05 to 0.2% by mass.
  • the abrasive composition When the abrasive composition is left standing in a bottle, the alumina abrasive grains settle, and when the abrasive composition is used again, it takes time to make it uniformly dispersed again.
  • the abrasive composition In polishing a sapphire substrate or the like, the abrasive composition is generally supplied in a circulating manner when the abrasive composition is supplied to a polishing machine. In this case, the alumina abrasive grains may settle in the abrasive composition flow path, the abrasive composition tank, or the transport tube, which may cause a reduction in the polishing rate.
  • a dispersion aid For the purpose of solving the problems such as sedimentation and re-dispersion as described above, a dispersion aid may be used in combination in the abrasive composition of the present invention.
  • the dispersion aid include alumina sol and celluloses. The reason why the dispersibility of the inorganic abrasive particles is improved by the addition of the dispersion aid is presumed to be because the abrasive particles are trapped in a chemical interaction network such as alumina sol or cellulose.
  • the alumina sol is a colloidal dispersion of aluminum hydroxide or hydrated alumina in an aqueous dispersion medium.
  • examples of the hydrated alumina include boehmite, pseudoboehmite, diaspore, dibsite, and bayerite.
  • Examples of the alumina sol in which aluminum hydroxide is colloidally dispersed in an aqueous dispersion medium include a sol product of an aluminum salt.
  • the aluminum salt solation product is obtained by reacting an aluminum salt with a substance that easily reacts with water to generate a hydroxyl group or a compound containing a hydroxyl group.
  • Examples of the aluminum salt used include aluminum sulfate, aluminum chloride, and aluminum nitrate.
  • Examples of substances that easily react with water and generate hydroxyl groups include ammonia, alkylamines, amine-based chelate compounds, aminocarboxylic acids, aminocarboxylic acid-based chelate compounds, and aminophosphonic acid-based chelate compounds.
  • Examples of the compound containing a hydroxyl group used include sodium hydroxide and potassium hydroxide.
  • Boehmite sol is obtained by solding boehmite and / or pseudo boehmite with an aluminum salt, an inorganic acid or an organic acid.
  • the aluminum salt used include aluminum sulfate, aluminum chloride, and aluminum nitrate.
  • Nitric acid, hydrochloric acid, etc. are mentioned as an inorganic acid used.
  • the organic acid used include acetic acid and gluconic acid.
  • boehmite sol one prepared by the above-mentioned method can be used, but a solidified boehmite sol that is commercially available can be dissolved in water at the time of use to produce a boehmite sol.
  • celluloses examples include cellulose, crystalline cellulose, carboxymethylcellulose, hydroxypropylmethylcellulose and the like.
  • alumina sol is preferable, and aluminum salt solation product and boehmite sol are more preferable.
  • the content of the dispersion aid is preferably 0.01 to 5% by mass with respect to the mass of the sapphire substrate polishing composition.
  • the amount is less than 0.01% by mass, the dispersion effect of the inorganic abrasive particles cannot be sufficiently obtained.
  • the amount is more than 5% by mass, an increase in the viscosity of the abrasive composition is observed, which hinders circulation use.
  • the content of the dispersion aid is more than 5% by mass, the polishing rate may be lowered.
  • the content of the dispersion aid is more preferably 0.01 to 2% by mass with respect to the mass of the abrasive composition for sapphire substrate.
  • the abrasive composition of the present invention may contain a pH adjusting agent in order to obtain a predetermined pH.
  • the pH adjuster include inorganic bases, organic bases, inorganic acids, organic acids and the like.
  • the inorganic base include sodium hydroxide, potassium hydroxide, ammonia and the like.
  • the organic base include tetramethylammonium hydroxide and alkanolamine.
  • the inorganic acid include sulfuric acid, nitric acid, phosphoric acid, hydrochloric acid and the like.
  • Examples of the organic acid include citric acid and malic acid.
  • the abrasive composition of the present invention includes a rust inhibitor, antibacterial agent, cleaning agent, surface modifier, scratch reducing agent, viscosity modifier, antifoaming agent, antioxidant, surfactant for other purposes, etc. Can also be used together as necessary.
  • the abrasive composition of the present invention can be prepared by mixing each component.
  • the abrasive composition of the present invention is an electronic component material such as an LED element, an optical component such as an optical filter, an electrically insulating material, a watch cover or window material, a sapphire substrate used as an abrasion resistant material, a glass substrate, It can be used for polishing a quartz substrate, silicon, a semiconductor substrate, or the like.
  • polishing agent composition The alumina particle used by an Example and a comparative example was prepared with the following method.
  • (Preparation example of alumina particles 1) A commercially available boehmite alumina (CA alumina manufactured by Sasol Co.) was calcined at 1160 ° C. for 9 hours so as to have a specific surface area BET of 4 m 2 / g. The crystal form of the alumina after firing was ⁇ -alumina. The fired product was wet-pulverized and adjusted to D50 of 0.45 ⁇ m. The specific surface area of the prepared alumina particles was BET 10 m 2 / g.
  • Example of preparation of alumina particles 2 Commercially available alumina (APA-0.4AF manufactured by Sasol Co., Ltd.) having a crystal form of ⁇ -alumina using boehmite alumina as a raw material was wet pulverized to adjust D50 to 0.35 ⁇ m.
  • the specific surface area of the prepared alumina particles was BET 11 m 2 / g.
  • D50 of the alumina particles was measured using a laser diffraction particle size distribution measuring machine (SALD2200, manufactured by Shimadzu Corporation).
  • SALD2200 laser diffraction particle size distribution measuring machine
  • the particle size distribution of the alumina particles is based on volume.
  • the specific surface area of the alumina particles was measured using a flow type specific surface area automatic measuring device (Shimadzu Corporation, Flowsorb II).
  • Alumina sol as a dispersion aid used in Examples and Comparative Examples was prepared by the following method.
  • (Preparation example of alumina sol 1) 77 g of commercially available boehmite alumina (CA alumina manufactured by Sasol Corporation), 44 g of aluminum chloride and 879 g of water were mixed and stirred with a homomixer to prepare a sol.
  • (Preparation example of alumina sol 2) 100 g of commercially available boehmite sol (Dispal 23N4-80 manufactured by Sasol Co.) was added to 888 g of water, and the mixture was thoroughly mixed and stirred to prepare a sol.
  • a polishing composition was prepared by the following method using sodium hexametaphosphate as a dispersion aid and the alumina sol prepared by the above method as a dispersion aid.
  • Example 1 Alumina particles 2 (D50: 0.35 ⁇ m, BET 11 m 2 / g), sodium aluminate and water were stirred and mixed so as to have the ratios in the table to prepare an abrasive composition. In addition, water was added so that it might become the remainder which remove
  • Example 2 Alumina particles 2 (D50: 0.35 ⁇ m, BET 11 m 2 / g), sodium aluminate, alumina sol 2 and water were stirred and mixed so as to have the ratios in the table to prepare an abrasive composition.
  • Example 3 An abrasive composition was prepared in the same manner as in Example 2. A polishing test was conducted using the obtained abrasive composition.
  • Example 4 Alumina particles 2 (D50: 0.35 ⁇ m, BET 11 m 2 / g), sodium aluminate, tetrapotassium salt of ethylenediaminetetraacetic acid (EDTA-4K), alumina sol 2 and water are stirred and mixed so that the proportions in the table are the same. Thus, an abrasive composition was prepared.
  • Example 5 Alumina particles 1 (D50: 0.45 ⁇ m, BET 10 m 2 / g), sodium aluminate, tetrasodium hydroxyethylidene diphosphonate (HEDP-4Na), sodium hexametaphosphate (hexameta), alumina sol 1 and water
  • HEDP-4Na tetrasodium hydroxyethylidene diphosphonate
  • alumina sol 1 water
  • the mixture was stirred and mixed to prepare an abrasive composition.
  • water was added so that it might become the remainder which remove
  • a polishing test was conducted using the obtained abrasive composition.
  • EDTA-4K ethylenediaminetetraacetic acid-tetrapotassium salt
  • HEDP-4Na hydroxyethylidene diphosphonic acid-tetrasodium salt
  • Hexmeta sodium hexametaphosphate
  • a sapphire substrate was polished under the following polishing conditions.
  • Polishing machine Air pressure 6B double-side polishing machine made by Speedfam Polishing pad: SUBA-800 Surface plate rotation speed: Lower 60rpm, Upper 20rpm Load: 120 g / cm 2 Polishing time: 420 minutes (7 hours) Abrasive composition supply amount: 120 ml / min Circulating polishing work: ⁇ 7.62 cm (3 inch) sapphire wafer ⁇ 3P
  • Polishing rate Polishing rate [ ⁇ m / hr] (mass before polishing of sapphire substrate ⁇ mass after polishing) [g] ⁇ polishing area of sapphire substrate [45 cm 2 ] ⁇ density of sapphire substrate [3.98 g / Cm 3 ] ⁇ polishing time [420 minutes] ⁇ 10000 [ ⁇ m / cm] ⁇ 60 [minute / hr], and shown in the table.
  • the surface roughness Ra of the sapphire substrate was measured with an atomic force microscope AFM (SPA-500 type manufactured by SII Technology) in a non-contact mode, a scan rate of 1.0 Hz, and a visual field of 10 ⁇ m 2 .
  • AFM atomic force microscope
  • Example 1 When Example 1 is compared with Comparative Example 1, and Examples 2 and 3 are compared with Comparative Example 2, it can be seen that a high polishing rate can be obtained by adding an oxoacid salt as a polishing accelerator. Comparing Example 4 with Examples 2 and 3, it can be seen that a higher polishing rate can be obtained when both a chelating compound and an oxoacid salt are included as polishing accelerators.
  • the present invention is an electronic component material such as an LED element, an optical component such as an optical filter, an electrically insulating material, a watch cover or window material, a sapphire substrate used as a wear resistant material, a glass substrate, a quartz substrate, silicon,
  • the present invention relates to an abrasive composition used for polishing a semiconductor substrate or the like.
  • the present invention is not limited to these applications, and can be used as an abrasive composition for other hard and brittle materials.
  • the abrasive composition of the present invention is a heat-resistant chip for laser emission, a substrate for LED lighting, a material for electronic components such as a substrate for high-frequency power devices used as GaN on Sapphire, a polarizer holding plate for a liquid crystal projector, a camera, etc.

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

Abstract

　L'invention concerne une composition d'agent de polissage destinée à un substrat en saphir, au moyen de laquelle une surface de polissage exempte de défauts de surface comme des rayures peut être obtenue avec une grande vitesse de polissage et une grande précision de polissage. La présente invention comprend comme constituants des particules de matériau inorganique de polissage, un accélérateur de polissage, et de l'eau. Les particules de matériau inorganique de polissage sont des particules d'alumine, et l'accélérateur de polissage est un sel d'oxoacide, le pH étant de 9,0 à 13,0. Le sel d'oxoacide est un sel de métal alcalin ou un sel de métal alcalino-terreux d'un oxoacide d'aluminium, de silicium ou de bore.
PCT/JP2015/075424 2014-09-16 2015-09-08 Composition d'agent de polissage pour substrat en saphir WO2016043089A1 (fr)

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JP2017105980A (ja) * 2015-09-25 2017-06-15 エア プロダクツ アンド ケミカルズ インコーポレイテッドＡｉｒ Ｐｒｏｄｕｃｔｓ Ａｎｄ Ｃｈｅｍｉｃａｌｓ Ｉｎｃｏｒｐｏｒａｔｅｄ ストップ‐オンシリコンコーティング層添加剤
WO2017170062A1 (fr) * 2016-03-31 2017-10-05 株式会社フジミインコーポレーテッド Composition pour polissage
JP2020057476A (ja) * 2018-09-28 2020-04-09 積水化学工業株式会社 電解質層、電極複合体及びリチウムイオン二次電池

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JP7457586B2 (ja) * 2020-06-18 2024-03-28 株式会社フジミインコーポレーテッド 研磨用組成物の濃縮液およびこれを用いた研磨方法

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JP2017105980A (ja) * 2015-09-25 2017-06-15 エア プロダクツ アンド ケミカルズ インコーポレイテッドＡｉｒ Ｐｒｏｄｕｃｔｓ Ａｎｄ Ｃｈｅｍｉｃａｌｓ Ｉｎｃｏｒｐｏｒａｔｅｄ ストップ‐オンシリコンコーティング層添加剤
US10144850B2 (en) 2015-09-25 2018-12-04 Versum Materials Us, Llc Stop-on silicon containing layer additive
JP2019049008A (ja) * 2015-09-25 2019-03-28 バーサム マテリアルズ ユーエス，リミティド ライアビリティ カンパニー ストップ‐オンシリコンコーティング層添加剤
WO2017170062A1 (fr) * 2016-03-31 2017-10-05 株式会社フジミインコーポレーテッド Composition pour polissage
JP2017179221A (ja) * 2016-03-31 2017-10-05 株式会社フジミインコーポレーテッド 研磨用組成物
CN108473851A (zh) * 2016-03-31 2018-08-31 福吉米株式会社 研磨用组合物
US11261346B2 (en) 2016-03-31 2022-03-01 Fujimi Incorporated Polishing composition
JP6096969B1 (ja) * 2016-04-26 2017-03-15 株式会社フジミインコーポレーテッド 研磨材、研磨用組成物、及び研磨方法
WO2017187689A1 (fr) * 2016-04-26 2017-11-02 株式会社フジミインコーポレーテッド Matériau abrasif, composition de polissage et procédé de polissage
JP2017197707A (ja) * 2016-04-26 2017-11-02 株式会社フジミインコーポレーテッド 研磨材、研磨用組成物、及び研磨方法
US10920104B2 (en) 2016-04-26 2021-02-16 Fujimi Incorporated Abrasive, polishing composition, and polishing method
JP2020057476A (ja) * 2018-09-28 2020-04-09 積水化学工業株式会社 電解質層、電極複合体及びリチウムイオン二次電池

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