WO2016204248A1 - 研磨砥粒、研磨スラリーおよび硬脆材の研磨方法、ならびに硬脆材の製造方法 - Google Patents

研磨砥粒、研磨スラリーおよび硬脆材の研磨方法、ならびに硬脆材の製造方法 Download PDF

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WO2016204248A1
WO2016204248A1 PCT/JP2016/067994 JP2016067994W WO2016204248A1 WO 2016204248 A1 WO2016204248 A1 WO 2016204248A1 JP 2016067994 W JP2016067994 W JP 2016067994W WO 2016204248 A1 WO2016204248 A1 WO 2016204248A1
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Prior art keywords
polishing
particles
alumina
hard
abrasive grains
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PCT/JP2016/067994
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English (en)
French (fr)
Japanese (ja)
Inventor
哲平 梶野
裕謙 尾崎
譲 齋藤
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住友化学株式会社
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Priority to JP2017524834A priority Critical patent/JP6792554B2/ja
Publication of WO2016204248A1 publication Critical patent/WO2016204248A1/ja

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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
    • B24B1/00—Processes of grinding or polishing; Use of auxiliary equipment in connection with such processes
    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B24—GRINDING; POLISHING
    • B24D—TOOLS FOR GRINDING, BUFFING OR SHARPENING
    • B24D3/00—Physical features of abrasive bodies, or sheets, e.g. abrasive surfaces of special nature; Abrasive bodies or sheets characterised by their constituents
    • 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 polishing abrasive grains used for polishing hard and brittle materials such as sapphire, polishing slurry, a method for polishing hard brittle materials, and a method for producing hard brittle materials.
  • a semiconductor layer such as gallium nitride (GaN) that is superior in characteristics to a silicon semiconductor in a high-frequency device such as a mobile phone, a light-emitting element such as an LED, and a power device such as a power conversion / control device.
  • a laminated semiconductor wafer in which a semiconductor substrate is laminated on a semiconductor forming substrate has been vigorously conducted. In such a laminated semiconductor wafer, if there are irregularities on the surface of the semiconductor forming substrate, the growth of the semiconductor layer becomes uneven or the bonding strength between the semiconductor forming substrate and the semiconductor layer becomes weak.
  • the substrate for use is required to have high surface smoothness.
  • polishing in the production of a semiconductor forming substrate, usually, rough polishing is performed by lapping, and then a scratch generated by lapping is removed by chemical mechanical polishing (CMP) as final polishing to obtain a highly smooth surface.
  • CMP is performed by pressing a polishing object against a wrap with a polishing pad and moving the polishing object and the wrap relative to each other while flowing a polishing slurry containing abrasive grains and an acid or alkali component.
  • the surface of the object to be polished is modified by the chemical components contained in the polishing slurry, and the mechanical polishing action by the polishing abrasive grains is increased to obtain a highly smooth polished surface.
  • Sapphire Al 2 O 3
  • silicon carbide SiC
  • gallium nitride GaN
  • aluminum nitride AlN
  • brittle materials having high hardness, that is, hard brittle materials, and are not easily processed by polishing as compared with conventional metal silicon and silicon oxide.
  • the hard brittle material generally means a hard and brittle material, and is a generic name for materials that are very hard materials such as glass, stone, or ceramics, but are weak against impact and easily cracked. Here, it has a Vickers hardness of 500 HV or more and may be broken when subjected to an impact.
  • CMP finish polishing
  • Patent Document 3 discloses a polishing slurry containing alumina abrasive grains having a specific particle size and proportion and having a pH in the range of 10.0 to 14.0. And it has been reported that by using alumina abrasive grains with strong alkalinity, an excellent polishing rate can be obtained as compared with colloidal silica abrasive grains.
  • Patent Document 4 discloses a polishing slurry containing alumina abrasive grains having a specific surface area and water and having a pH of 8.5 or more.
  • the present invention provides the following means.
  • Abrasive abrasive used for polishing hard and brittle materials comprising abrasive particles having one or more neck portions, and an alumina powder having a mass average particle diameter of 3 ⁇ m or less grain.
  • ⁇ 4> In the alumina powder having a particle diameter of 0.5 to 2 times the mass average particle diameter, the number ratio of the connected particles is 20% or more, and any one of ⁇ 1> to ⁇ 3> Abrasive grains.
  • ⁇ 5> In the alumina powder having a particle size of 0.5 to 2 times the mass average particle size, the number ratio of the particles having a surface index of 1.4 or more is 25% or more.
  • ⁇ 1> to ⁇ 4> The abrasive grain in any one.
  • a polishing slurry comprising the polishing abrasive grain according to any one of ⁇ 1> to ⁇ 5> and water or a solvent mainly containing water and having a pH of 12 or more.
  • a method for polishing a hard and brittle material including a step of chemically mechanically polishing a surface of the hard and brittle material using the polishing slurry according to ⁇ 6>.
  • a method for producing a hard and brittle material comprising a step of polishing the hard and brittle material by the polishing method according to ⁇ 7>.
  • the method for producing a hard and brittle material according to ⁇ 8>, wherein the hard and brittle material to be polished is sapphire.
  • a polishing abrasive, a polishing slurry, and a method for polishing a hard and brittle material that can achieve both a high polishing speed and surface smoothness in polishing a hard and brittle material.
  • Example 2 It is a SEM image of the abrasive grain of Example 2 used for image analysis. It is a SEM image of the abrasive grain of Example 2 used for image analysis.
  • 2 is an SEM image of the abrasive grains of Example 1.
  • 3 is a SEM image of polishing abrasive grains of Example 2.
  • 4 is a SEM image of polishing abrasive grains of Example 3.
  • 4 is a SEM image of the abrasive grains of Example 4.
  • 6 is a SEM image of polishing abrasive grains of Example 5.
  • 2 is a SEM image of the abrasive grains of Comparative Example 1.
  • the abrasive grains of the present invention are abrasive grains used for polishing hard and brittle materials, contain connected particles having one or more neck portions, and have an average particle diameter of 3 ⁇ m or less. It is. Although the abrasive grains of the present invention can be used as they are, they are usually dispersed in a solvent (dispersion medium) and supplied to a polishing apparatus as a polishing slurry. The details of the polishing slurry containing the abrasive grains of the present invention and the polishing method using the polishing slurry will be described later.
  • polishing abrasive grain according to the present invention contains connected particles having one or more neck portions to improve the polishing rate and the surface smoothness of the object to be polished is detailed at this stage.
  • the reason is not completely clear, but when the shape of alumina has a neck portion, it becomes easier to be held by the polishing pad used in CMP, and the number of abrasive grains actually acting on the polishing increases and polishing is performed.
  • One of the causes is presumed to be an increase in speed.
  • connected particles having one or more neck portions means that a plurality of primary particles are connected by sintering or the like, or the primary particles themselves are concave and convex and are concave portions. It means a particle having one or more neck portions.
  • Examples of the method for determining whether or not the particles are connected particles having one or more neck portions include the following [Determination Method 1] and [Determination Method 2].
  • a particle that satisfies one of the determination criteria of [Determination Method 1] and [Determination Method 2] is a connected particle having one or more neck portions.
  • Alumina particles are observed with a scanning electron microscope (SEM) at a magnification of 20000 times, the presence or absence of a neck portion is visually determined, and alumina particles having one or more neck portions are separated by one or more neck portions. The connected particles are determined.
  • SEM scanning electron microscope
  • the area defect rate is preferably 15% or more.
  • the area defect rate is usually 40% or less.
  • the area defect rate may be calculated by image analysis using commercially available image analysis software such as “WinROOF” of Mitani Corporation.
  • FIG. 1 is an SEM image in which alumina particles of Example 2 described later are dispersed.
  • FIG. 4 is an SEM image in which alumina particles are gathered.
  • FIG. 1 to 4 in FIG. 1 are in contact with or overlapping two or more alumina particles, and 5 is one alumina particle.
  • the contour and the number of the lower particles are unclear. Only the uppermost particle surrounded by is determined as one alumina particle and is set as an analysis target.
  • FIG. 2 among the alumina particles shown in FIG. 1, a particle determined as one alumina particle is filled, and the filled particle is an analysis target.
  • the number ratio of the connected particles having one or more neck portions is preferably 20% or more of the total number of particles constituting the alumina powder, and preferably 50% or more. More preferably, it is more preferably 70% or more.
  • the number ratio of the connected particles having one or more neck portions is large, the ratio of particles contributing to polishing in the alumina abrasive grains increases, and the polishing rate can be further increased.
  • the abrasive grains of the present invention are the number of connected particles having one or more neck portions in an alumina powder having a particle diameter of 0.5 to 2 times the mass average particle diameter of the alumina powder.
  • the ratio is preferably 20% or more, more preferably 25% or more, and further preferably 30% or more.
  • the number ratio is, for example, the alumina particles 100 having a particle diameter of 0.5 to 2 times the mass average particle diameter of the alumina powder in the SEM image obtained by observing the alumina particles dispersed as described above at a magnification of 20000 times. Randomly extracting the particles, as described above, calculating the area defect rate of each particle to determine whether it is a connected particle having one or more neck parts, and obtain by the following formula Can do.
  • the particle diameter of the alumina powder may be the equivalent circle diameter of the SEM image of the alumina particles, and may be calculated by image analysis using commercially available image analysis software such as “WinROOF” of Mitani Corporation.
  • Number ratio of connected particles having one or more neck portions (%) in alumina powder having a particle diameter of 0.5 to 2 times the mass average particle diameter of alumina powder (Number of particles having an area defect rate of 10% or more having a particle diameter of 0.5 to 2 times the mass average particle diameter of alumina powder) / (0.5 to the mass average particle diameter of alumina powder extracted at random) Total number of particles having a double particle size (100 particles)) ⁇ 100 (III)
  • the abrasive grains of the present invention preferably contain particles having a surface index of 1.4 or more, more preferably 1.5 or more, from the viewpoint of obtaining a superior polishing rate.
  • the upper limit of the surface index of the particles contained in the abrasive grains of the present invention is usually 3.5.
  • the reason why the polishing rate is improved by containing particles having a surface index of 1.4 or more and the surface smoothness of the object to be polished is improved is not completely clear at this stage. If the surface index of the particles is 1.4 or more, the fine irregularities on the surface of the particles are large, which increases the number of minute contact points between the polishing substrate and abrasive grains used in CMP and improves the polishing rate. Presumed to be one. Further, by setting the surface index to 3.5 or less, it is effective in excluding particles that do not contribute to the polishing rate but have a high surface index, for example, very elongated flat particles.
  • the surface index of alumina particles is 1 when the cross section is a perfect circle (three-dimensionally a sphere), and is an index that indicates the distance from the surface, and is lower than the circumference and area of the alumina particles.
  • Surface index (square of perimeter of alumina particles) / (area of alumina particles) / 4 ⁇ (IV)
  • the surface index of the alumina particles may be calculated, for example, by observing the alumina particles with a SEM at a magnification of 20000 times and the circumference and area of the SEM image of the alumina particles.
  • the surface index may be calculated by image analysis using commercially available image analysis software such as “WinROOF” of Mitani Corporation. At the time of image analysis, as described above, an SEM image in which alumina particles are dispersed is obtained so that one alumina particle can be observed, and a particle determined as one alumina particle is set as an analysis target.
  • fine particles generated by pulverization or the like and coarse particles not pulverized have a small contribution to the polishing action. Therefore, it is preferable to obtain the surface index using alumina particles that have a large contribution to the polishing action excluding such particles as a measurement target. Therefore, in a preferred embodiment, it is preferable to measure alumina particles having a particle diameter of 0.5 to 2 times the mass average particle diameter of the alumina powder, and the surface index of the alumina particles to be measured has a surface index of 1. .4 or more is preferable.
  • the abrasive grains of the present invention the alumina powder having a particle diameter of 0.5 to 2 times the mass average particle diameter of the alumina powder, the number ratio of particles having a surface index of 1.4 or more, It is preferably 25% or more, more preferably 30% or more, and further preferably 35% or more.
  • the number ratio is large, the ratio of particles contributing to polishing in the alumina abrasive grains increases, and the polishing rate can be further increased.
  • the number ratio is, for example, the alumina particles 100 having a particle diameter of 0.5 to 2 times the mass average particle diameter of the alumina powder in the SEM image obtained by observing the alumina particles dispersed as described above at a magnification of 20000 times. Individually extracted pieces, the surface index of each particle is calculated, and can be obtained by the following formula.
  • the particle diameter of the alumina powder may be the equivalent circle diameter of the SEM image of the alumina particles, and may be calculated by image analysis using commercially available image analysis software such as “WinROOF” of Mitani Corporation.
  • Number ratio of particles having surface index of 1.4 or more in alumina powder having a particle size of 0.5 to 2 times the mass average particle size of alumina powder (Number of particles having a surface index of 1.4 or more having a particle size of 0.5 to 2 times the mass average particle size of alumina powder) / (0.5 to the mass average particle size of alumina powder extracted randomly) Total number of particles having a double particle size (100 particles)) ⁇ 100 (V)
  • the average particle size of the alumina powder is 3 ⁇ m or less, preferably 2 ⁇ m or less.
  • the “average particle size” defined here means a particle size corresponding to a cumulative percentage of 50% on a mass basis obtained by a laser diffraction method. If the particle size of the alumina powder, which is an abrasive grain, exceeds 3 ⁇ m, a highly smooth surface may not be obtained.
  • the lower limit of the average particle diameter of the alumina powder is not limited in terms of obtaining a highly smooth surface, but since the polishing rate decreases as the particle diameter decreases, it is usually 0.1 ⁇ m or more, preferably 0.2 ⁇ m or more. It is.
  • Alumina has crystal forms such as ⁇ -alumina and ⁇ -alumina, but ⁇ -alumina is preferable for high-speed polishing of hard and brittle materials.
  • ⁇ -alumina ⁇ -alumina having an alkali resistance of 0.7 or more is preferable.
  • the “degree of alkali resistance” is an index of how much the ⁇ -alumina crystal structure is maintained when immersed in a highly alkaline solution for a certain period of time, specifically measured by an X-ray diffraction pattern. It is defined by the peak intensity ratio before and after immersion in the alkaline solution. A specific method for defining the alkali resistance will be described later in Examples.
  • ⁇ -alumina means alumina whose main phase of crystal phase is ⁇ -phase. Therefore, it may contain a ⁇ phase, a ⁇ phase, a ⁇ phase, a ⁇ phase, a ⁇ phase, or a ⁇ phase, which is a general crystal phase as alumina.
  • the method for producing the alumina powder is not particularly limited.
  • a method of firing aluminum hydroxide produced by the Bayer method a method of firing aluminum hydroxide produced by the aluminum alkoxide method; a method of synthesizing using organic aluminum
  • a method in which transition alumina or an alumina powder that becomes transition alumina by heat treatment is fired in an atmosphere gas containing hydrogen chloride as a raw material JP-A-11-049515, JP-A-2010-150090, JP-A-2008 And the methods described in JP-A No. 19033, JP-A No. 2002-047009, JP-A No. 2001-354413, and the like.
  • the abrasive grains have a shape having an edge due to a fracture surface or the like (a shape with sharp corners) because scratches are likely to remain on the polished surface of the object to be polished.
  • fine aluminum hydroxide it is possible to strengthen the cohesion between particles in the process of particle growth by firing, etc., and the connection part (neck part) strength of the connected particles is excellent, and the edge is caused by the neck fracture surface, etc.
  • the ⁇ -alumina particles have a small amount, and there is an advantage that no scratches remain on the polished surface of the object to be polished and the finish is not impaired.
  • aluminum alkoxide method for example, aluminum alkoxide is hydrolyzed with water to obtain slurry, sol, or gel aluminum hydroxide, and dried to obtain dry powdered aluminum hydroxide.
  • the method of obtaining is mentioned.
  • the powdered aluminum hydroxide obtained by drying is a bulky powder whose light bulk density is usually about 0.1 to 0.4 g / cm 3 , preferably 0.1 to 0.2 g / cm 3 . Has light bulk density.
  • the cumulative pore volume of aluminum hydroxide (pore radius in the range of 0.01 ⁇ m or more and 1 ⁇ m or less) is not particularly limited, but preferably has a cumulative pore volume of 0.6 mL / g or more.
  • Such aluminum hydroxide has small primary particles, excellent dispersibility, and few aggregated particles. Therefore, even when baked, it is possible to prevent generation of alumina aggregated particles that are firmly bonded and difficult to grind.
  • the target ⁇ -alumina powder can be obtained by firing dry powdered aluminum hydroxide obtained by the aluminum alkoxide method.
  • the baking of aluminum hydroxide is usually performed by filling a baking vessel with aluminum hydroxide.
  • a baking container a sheath etc. are mentioned, for example.
  • the material of the firing container is preferably alumina from the viewpoint of preventing contamination of the ⁇ -alumina powder to be obtained, and particularly preferably high-purity ⁇ -alumina.
  • the method of filling aluminum hydroxide into the baking container is not particularly limited, but it is preferable that the aluminum hydroxide is filled with its own weight and not excessively compacted.
  • a firing furnace used for firing aluminum hydroxide for example, a stationary material firing furnace represented by a tunnel kiln, a batch-type aerated flow box firing furnace, a batch-type parallel flow box firing furnace, and the like; And a material transfer type firing furnace.
  • the calcining temperature of aluminum hydroxide, the heating rate up to the calcining temperature, and the calcining time are appropriately selected so as to obtain ⁇ -alumina having desired physical properties.
  • the calcining temperature of aluminum hydroxide is, for example, 1100 ° C. or higher and 1450 ° C. or lower, preferably 1200 ° C. or higher and 1350 ° C. or lower.
  • the rate of temperature rise when heating to this calcining temperature is usually 30 ° C./hour or higher and 500 ° C./hour.
  • the baking time of aluminum hydroxide is usually 0.5 hours or more and 24 hours or less, preferably 1 hour or more and 10 hours or less.
  • aluminum hydroxide may be baked in an air atmosphere or in an inert gas atmosphere such as nitrogen gas or argon gas. May be fired in a high atmosphere.
  • the obtained alumina powder may be agglomerated in a state where the average particle diameter exceeds 10 ⁇ m. In that case, it grind
  • the pulverization of the alumina powder can be performed using a known apparatus such as a vibration mill, a ball mill, or a jet mill, and any of a dry pulverization method and a wet pulverization method can be employed.
  • a method of grinding without using a grinding medium such as a ball for example, grinding with a jet mill
  • a pulverizing medium such as a ball or a bead
  • a method of pulverizing while maintaining the neck portion while adjusting the conditions so as not to include coarse aggregated particles for example, a vibration mill is preferable.
  • the content of coarse particles of 10 ⁇ m or more contained in the obtained alumina powder is preferably 10 ppm or less, and more preferably 3 ppm or less.
  • [(D100 ⁇ d5) ⁇ mass average particle diameter] is 30 or less when the particle diameters corresponding to the cumulative percentage of 5% and the cumulative 100% are d5 and d100, respectively, from the small diameter side of the particle size distribution of the alumina powder. Preferably, it is 10 or less.
  • the surface in contact with ⁇ -alumina is made of a high-purity alumina material or is resin-lined in that the resulting alumina powder is less contaminated with foreign matters.
  • the pulverizing media used for this is also made of a high-purity alumina material.
  • the polishing slurry of the present invention contains the polishing abrasive grain of the present invention and water or a solvent mainly composed of water, and has a pH of 12 or more.
  • the polishing slurry of the present invention is a strong alkali having a pH of 12 or more, when the slurry is used, the surface of the hard and brittle material to be polished is modified, and the polishing of the present invention having excellent polishing properties in that state. Since it is physically polished by the abrasive grains, a high polishing rate can be obtained.
  • the pH of the polishing slurry is important not only for modifying the surface of the object to be polished, but also for controlling the dispersibility of the abrasive grains when water or a solvent mainly composed of water is used.
  • a suitable pH range is determined in consideration of the type of abrasive grains and their alkali resistance and dispersibility.
  • the pH is 12 or more, preferably 13 or more.
  • ⁇ -alumina having an alkali resistance of 0.7 or more as a polishing abrasive, it is stored for a long time in a slurry having a pH of 12 or more, and even when used, deterioration of the polishing abrasive is suppressed, and excellent polishing. The action can be kept.
  • the concentration of the abrasive grains in the polishing slurry may be determined within a concentration range in which the abrasive grains can be stably dispersed in the polishing slurry, and is usually 0.1 to 50% by weight, preferably 5 to 20% by weight. It is.
  • the solvent is a medium for dispersing and dissolving the abrasive grains and optional components added as necessary.
  • water or a solvent mainly composed of water is used.
  • the “solvent mainly composed of water” means a solvent containing at least 50% by weight of water and containing other solvents such as ethanol or additional components in addition to water.
  • Distilled water and ion-exchange water are preferable at the point of the influence with respect to a mixing
  • the alkali component is added to the slurry for pH adjustment, and is not particularly limited as long as the effects of the present invention are not impaired. Specifically, the alkali metal hydroxide of sodium hydroxide, potassium hydroxide, lithium hydroxide or the like is used. Products, hydroxides of tetraalkylammonium, hydroxides of alkaline earth metals such as calcium hydroxide or magnesium hydroxide, ammonium hydroxide and the like. Among these, sodium hydroxide and potassium hydroxide are preferably used from the viewpoint of availability and cost.
  • the polishing slurry of the present invention can appropriately contain other components as needed as long as the purpose of the present invention is not impaired in addition to the alkali component.
  • examples of other components include a dispersant, a surfactant, and a viscosity modifier. When these other components are used, the content is usually in the range of 0.01 to 10% by mass with respect to the total mass of the abrasive grains.
  • dispersant examples include condensed phosphoric acid or condensed phosphate, polystyrene sulfonate, polycarboxylic acid type polymer compound, polyacrylic acid type polymer compound, polyoxyethylene sorbitan fatty acid ester, polyoxyethylene sorbitol fatty acid ester, and the like.
  • Surfactants include anionic surfactants, nonionic surfactants, cationic surfactants, and amphoteric surfactants.
  • the viscosity modifier include water-soluble cellulose ethers, polysaccharides, polyhydric alcohols and derivatives thereof, water-soluble polymer compounds, water-soluble oxides having a thickening action and salts thereof, and biopolymers.
  • the polishing slurry is prepared by mixing polishing abrasive grains (and optional components) so as to be uniformly dispersed in a dispersion medium.
  • the mixing method is not particularly limited, and examples thereof include a stirring and mixing method using an ultrasonic disperser, a homogenizer, and the like.
  • the mixing method can be performed by a conventionally known mixing method, the mixing order is also arbitrary, and any two components of the constituents of the polishing slurry (polishing abrasive grains, alkali component, solvent, and optional components) or Three or more components may be mixed in advance, and then the remaining components may be mixed, or all may be mixed at once.
  • the method for polishing a hard and brittle material of the present invention uses the above-described polishing slurry of the present invention to chemically and mechanically polish (CMP) the surface of the hard and brittle material.
  • CMP chemically and mechanically polish
  • the polishing method of the present invention is the same as the conventional polishing method by CMP except that the polishing slurry of the present invention is used as the polishing slurry.
  • polishing can be performed.
  • the hard and brittle material to be polished in the polishing method of the present invention include aluminum oxide (sapphire), diamond, silicon carbide, boron carbide, zirconium carbide, tungsten carbide, silicon nitride, titanium nitride, gallium nitride, and aluminum nitride.
  • Etc Any of single crystal, polycrystalline, and amorphous can be polished.
  • sapphire especially single crystal sapphire
  • suitable as a substrate of a semiconductor element is a hard and brittle material that is difficult to process, and improvement in productivity by high-speed polishing has been demanded. Therefore, the polishing method of the present invention is preferable. It is a target.
  • the surface of the hard and brittle material after polishing is preferably smoother.
  • the arithmetic average surface roughness (Ra) is preferably 2 nm or less, preferably 1 nm. It is more preferable to make it below. However, this is not limited to the case where the surface roughness is not so required, for example, when polishing is performed using another abrasive grain.
  • polishing apparatus a conventionally known CMP polishing apparatus can be used.
  • a case where a general single-side polishing type CMP polishing apparatus is used will be described.
  • a typical configuration of a single-side polishing type CMP polishing apparatus is a state in which a polishing plate is rotated around a rotation axis, a polishing pad is attached to the surface, and an object to be polished is fixed to the lower part of the sample holder with wax or the like.
  • a sample holder (hereinafter sometimes referred to as a head) that can be pressed against the polishing pad, a pressurizing mechanism for polishing load, and a nozzle that supplies polishing slurry containing polishing grains on the polishing pad. It is provided as a main component.
  • the polishing plate is supplied from the nozzle to the surface of the polishing pad affixed to the surface plate in a state where the surface plate and the sample holder are rotated around their respective axis centers.
  • the surface to be polished of the object to be polished is polished by pressing the object to be polished held on the lower surface against the polishing pad.
  • Polishing speed (polishing slurry (type of abrasive grains, particle diameter, concentration of abrasive grains in the polishing slurry, supply speed of slurry)) polishing apparatus (polishing load, rotation speed of surface plate and head, type of polishing pad) Determined by. Since the polishing slurry of the present invention having the above-described properties is used, a high polishing rate can be set even for a substrate made of a hard and brittle material (particularly a single crystal sapphire substrate), and a highly smooth surface. Can be produced efficiently.
  • the polishing speed capable of maintaining the surface roughness (Ra) of the substrate of 1 nm. can be 4 ⁇ m / hr or more (preferably 5 ⁇ m / hr or more, more preferably 6 ⁇ m / hr or more).
  • polishing pads such as non-woven fabrics, polyurethane foams, porous resins, and non-porous resins, which can be used on the surface plate, and those that are generally available on the market can be used. What is necessary is just to determine suitably considering grinding conditions, such as a diameter, grinding
  • the supply amount of the polishing slurry is appropriately determined in consideration of the constituent material of the object to be polished, the type of polishing abrasive grains, and the polishing abrasive grain concentration in the slurry.
  • the abrasive grains do not necessarily have to be supplied to the polishing pad as a polishing slurry in which all components are mixed in advance.
  • the abrasive grains may be supplied as they are and the solvent may be supplied separately.
  • the number of rotations of the platen during polishing is not particularly limited, and may be a range that can be stably operated within the range of the capability of the polishing apparatus to be used.
  • the rotation speed of the surface plate is fast, but it is determined appropriately in consideration of the polishing abrasive grains (polishing slurry) to be used and the surface smoothness required for the object to be polished. It is preferable.
  • the load at the time of polishing is not particularly limited, and may be determined within a range where the polishing apparatus used can be stably operated. In order to perform polishing in a short time, it is preferable that the load is large. However, since the power load of the motor for rotation is also large, the polishing abrasive grains (polishing slurry) to be used, and the surface smoothness required for the object to be polished, etc. It is preferable to determine appropriately.
  • the polishing slurry used for polishing the object to be polished may be recovered and reused.
  • the waste liquid is reduced, so that the environmental load can be reduced and the cost can be reduced.
  • consumed components polishing abrasive grains, solvent, pH adjuster, and other optional components
  • the polishing method of the present invention has been described in the case of using a general single-side polishing type CMP polishing apparatus.
  • the polishing apparatus disclosed this time operating conditions and various parameters not explicitly disclosed, The dimensions, weight, volume, and the like of the components do not deviate from the range normally practiced by those skilled in the art, and values that can be easily assumed by those skilled in the art are adopted.
  • the polishing apparatus used in the polishing method of the present invention is not limited to a single-side polishing type CMP polishing apparatus.
  • a double-side polishing type polishing apparatus or an apparatus that reciprocates the sample holder instead of rotating it may be used.
  • the surface plate does not perform a rotational movement, and may be a belt type that moves in one direction, for example.
  • the method for producing a hard and brittle material of the present invention includes a step of polishing the hard and brittle material by the polishing method of the present invention (hereinafter referred to as “the polishing step of the present invention”). Since the manufacturing method of the present invention includes the polishing step of the present invention described above, a hard and brittle material having a highly smooth surface with high productivity can be manufactured.
  • the steps other than the step of polishing the hard and brittle material in the polishing step of the present invention may be performed according to a known method for producing a hard and brittle material as a raw material.
  • sapphire especially a single crystal sapphire substrate
  • sapphire substrate which is a suitable target for the method for producing a hard and brittle material of the present invention will be described as an example.
  • Sapphire especially single-crystal sapphire
  • the sapphire crystal has different properties depending on the plane orientation, and the c-plane which is a polar plane and the r-plane which is a semipolar plane are used as a semiconductor substrate for growing a semiconductor layer such as gallium nitride on the surface.
  • the a-plane and m-plane which are nonpolar surfaces, are suitable for applications, and are suitable for applications requiring a substrate having high hardness and no scratches (for example, a substrate for a thin film or a chamber window for a semiconductor manufacturing apparatus).
  • a sapphire crystal (ingot) is ground to an appropriate size and cut to obtain a cut piece of a predetermined size (grinding / cutting step).
  • plate-like sapphire is obtained by carrying out plane cutting of the obtained cut piece to predetermined thickness (plane cutting process).
  • the obtained plate-like sapphire is roughly polished by lapping or the like, and scratches generated by lapping are removed by CMP, which is finish polishing, to obtain a highly smooth surface.
  • CMP finish polishing
  • the method for producing a hard and brittle material of the present invention can be applied to the production of a hard and brittle material that is reused by removing the semiconductor layer from a product containing the hard and brittle material, for example, a wafer on which the semiconductor layer is formed. Good.
  • the portion other than the hard and brittle material is removed from the product containing the hard and brittle material by grinding or rough polishing, and then subjected to the polishing step of the present invention.
  • the method for producing a hard and brittle material of the present invention may further include an optional step as needed.
  • an optional step for example, a heat treatment process, a wet etching process, a cleaning process, and the like can be given.
  • the heat treatment method in the heat treatment step is not particularly limited, and may be performed by a conventionally known method as a heat treatment method of the target hard and brittle material.
  • Examples of the purpose of performing the heat treatment include removing crystal distortion remaining inside the hard and brittle material, or facilitating oxidation of the surface of the hard and brittle material to facilitate surface processing.
  • the heat treatment conditions such as the heat treatment temperature and the heat treatment atmosphere are appropriately determined according to the type or purpose of the hard brittle material to be treated.
  • the wet etching method in the wet etching step is not particularly limited, and may be performed by a conventionally known method as a wet etching method for a target hard and brittle material.
  • Wet etching conditions such as the type of chemical used for wet etching, the processing temperature, and the processing time are appropriately determined depending on the material of the hard brittle material to be processed or the object to be removed.
  • the cleaning method in the cleaning step is not particularly limited, and may be performed by a conventionally known method as a method for cleaning the target hard and brittle material.
  • hard brittle materials to be cleaned can be obtained by using an organic solvent such as alcohol, or an acid cleaning solution such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, hydrofluoric acid, hydrogen peroxide, alkali hydroxide, ammonia, organic amine. It is possible to remove a trace amount of foreign matters remaining on the substrate by rinsing with a basic cleaning solution such as the above or immersing in a cleaning solution.
  • the use of the manufactured hard and brittle material may be appropriately selected depending on the type of other hard and brittle material.
  • a substrate for a GaN-based semiconductor layer used for a high-frequency device, an LED light-emitting element, or the like, or a polarizer holding substrate for a liquid crystal projector can be used.
  • Example 1 Evaluation of number ratio of connected particles having one or more neck portions Example 1 was evaluated by [Evaluation Method 1] described later, and Examples 2 to 5 and Comparative Example 1 were evaluated by [Evaluation] described later. Evaluation was made by method 2].
  • the number ratio of the connected particles having one or more neck portions of the alumina particles is determined by observing the aggregated state of the alumina particles at a magnification of 20000 with a SEM, and a total of 100 particles are randomly selected from the SEM image. Extraction was performed, and the presence or absence of a neck portion was judged visually for each particle, and the calculation was performed according to the following formula. In the evaluation method 1, in the SEM image, even in the case of connected particles having a neck portion, the neck portion may not be confirmed depending on the observation angle or the arrangement state of the particles. Only particles visually confirmed to have a part were calculated as “connected particles having a neck part”.
  • Number ratio of connected particles having one or more neck parts (Number of particles visually confirmed to have a neck portion) ⁇ (Total number of particles randomly extracted (100 particles)) ⁇ 100 (II)
  • number ratio [1] the number ratio may be referred to as “number ratio [1]”.
  • alumina particles are not dispersed to the extent shown in FIG. 1
  • a diluted solution obtained by diluting the suspension twice with ethanol is prepared, and the degree of dispersion of alumina particles is adjusted in the same manner as described above. The same operation was repeated until the aluminum particles were dispersed to the extent shown in FIG.
  • the SEM image of the resulting alumina particles was analyzed using “WinROOF” from Mitani Shoji Co., Ltd., and 100 alumina particles with an equivalent circle diameter of 0.5 to 2 times the mass average particle diameter were randomly created. Extracted into. When two or more alumina particles contacted or overlapped, only the uppermost particle was determined as one alumina particle and extracted.
  • the area defect rate of each particle is calculated to determine whether it is a connected particle having one or more neck portions, and the mass of the alumina powder
  • the number ratio of connected particles having one or more neck portions in alumina powder having a particle size of 0.5 to 2 times the average particle size was calculated by the following formula.
  • Number ratio of connected particles having one or more neck portions (%) in alumina powder having a particle diameter of 0.5 to 2 times the mass average particle diameter of alumina powder (Number of particles having an area defect rate of 10% or more having a particle diameter of 0.5 to 2 times the mass average particle diameter of alumina powder) / (0.5 to the mass average particle diameter of alumina powder extracted at random) Total number of particles having a double particle size (100 particles)) ⁇ 100 (III)
  • the number ratio may be referred to as “number ratio [2]”.
  • Number ratio of particles having surface index of 1.4 or more in alumina powder having a particle size of 0.5 to 2 times the mass average particle size of alumina powder (Number of particles having a surface index of 1.4 or more having a particle size of 0.5 to 2 times the mass average particle size of alumina powder) / (0.5 to the mass average particle size of alumina powder extracted randomly) Total number of particles having a double particle size (100 particles)) ⁇ 100 (V)
  • the number ratio may be referred to as “number ratio [3]”.
  • Mass average particle diameter A laser particle size distribution measuring apparatus ["MICROTRACK” manufactured by Nikkiso Co., Ltd.] was used, and the particle diameter corresponding to a cumulative percentage of 50% on the mass basis was defined as the average particle diameter. Further, the particle diameters corresponding to the cumulative percentage of 5% and the cumulative 100% on the mass basis from the small diameter side of the particle size distribution were d5 and d100, respectively. In the measurement, ultrasonic dispersion was performed with a 0.2 wt% sodium hexametaphosphate aqueous solution, and the refractive index of the alumina particles was 1.76.
  • Alkali Tolerance Alumina powder was added to an aqueous solution adjusted to pH 13.5 with potassium hydroxide (KOH) so that the solid concentration was 10% by weight, and the solid components after immersion for 4 weeks were recovered.
  • KOH potassium hydroxide
  • BET specific surface area As a specific surface area measuring device, “Flowsorb II 2300” manufactured by Shimadzu Corporation is used, and specified in JIS-Z-8830: 2013 “Specific surface area measuring method of powder (solid) by gas adsorption”. In accordance with the determined method, the BET specific surface area was determined by a single point method of nitrogen adsorption.
  • Example 1 Production of abrasive grains
  • Aluminum isopropoxide prepared from aluminum having a purity of 99.99% is hydrolyzed with water to obtain slurry aluminum hydroxide, which is then dried.
  • dry powder aluminum hydroxide having a light bulk density of 0.1 g / cm 3 was obtained.
  • this dried powdery aluminum hydroxide is calcined by being held at 1220 ° C. for 4 hours in a gas furnace that is calcined by combustion of propane gas or the like, and is pulverized by a jet mill and is made of ⁇ -alumina powder.
  • An abrasive grain was obtained.
  • FIG. 3 shows an SEM image of the abrasive grains ( ⁇ -alumina powder) of Example 1 in a state where the alumina particles are aggregated.
  • polishing abrasive grains of Example 1 were added to an aqueous solution adjusted to pH 13.5 with potassium hydroxide (KOH) so that the solid concentration was 10% by weight, and blade stirring was performed. Later, the polishing slurry of Example 1 was obtained by irradiating ultrasonic waves and dispersing the abrasive grains for 1 hour.
  • KOH potassium hydroxide
  • polishing sample a sapphire substrate (c-plane): 2 inch ⁇ (dialap-processed, Ra 5 nm) was used.
  • a polishing apparatus NANO-450-DOCAb manufactured by Hi-Technos Co., Ltd. was used, and the slurry of Example 1 was used for polishing for 1 hour under the following conditions.
  • the average polishing rate was determined from the weight difference of the sapphire substrate before and after polishing. The surface of the sample after calculation and polishing was observed with an optical microscope (50 times).
  • Example 1 the average polishing rate was 6.5 ⁇ m / hour, the sample surface after polishing was extremely flat, and scratches observed before polishing were not observed.
  • Example 2 (1) Production of abrasive grains Under the same conditions as Example 1, abrasive grains of Example 2 were obtained. About the obtained abrasive grain ( ⁇ alumina powder), the method (1) [Evaluation Method 2] is used to evaluate the number ratio [2] of connected particles having one or more neck portions, and the above method ( From 2) to (5), the surface index, mass average particle diameter, alkali resistance, and BET specific surface area were evaluated. The evaluation results are shown below.
  • FIG. 4 shows an SEM image of the abrasive grains ( ⁇ -alumina powder) of Example 2 in a state where the alumina particles are aggregated.
  • polishing slurry of Example 2 was obtained in the same manner as Example 1 except that the polishing abrasive grain of Example 2 was used instead of the polishing abrasive grain of Example 1.
  • polishing test A sapphire substrate (c-plane): 2 inch ⁇ (dialap processed, Ra 5.8 nm) is used as a polishing sample, and the polishing slurry of Example 2 is used instead of the polishing slurry of Example 1.
  • a polishing test was conducted in the same manner as in Example 1 except that. In Example 2, the average polishing rate was 6.5 ⁇ m / hour, the sample surface after polishing was extremely flat, and scratches observed before polishing were not observed. Moreover, as a result of evaluating surface roughness by the said method (6), surface roughness was 1.0 nm.
  • Example 3 As abrasive grains of Example 3, dry powdered aluminum hydroxide obtained by the same method as in Example 1 is held at 1200 ° C. for 3 hours in a gas furnace that is fired by combustion of propane gas or the like. An alumina powder having the following physical properties obtained by firing and grinding with a vibration mill was used. For the abrasive grains, the number ratio [2] of connected particles having one or more neck portions is evaluated by the above method (1) [Evaluation method 2], and by the above methods (2) to (5). The surface index, the mass average particle diameter, the alkali resistance, and the BET specific surface area were evaluated. The evaluation results are shown below. FIG.
  • polishing slurry of Example 3 was obtained in the same manner as Example 1 except that the polishing abrasive grain of Example 3 was used instead of the polishing abrasive grain of Example 1.
  • polishing Test A polishing test was conducted in the same manner as in Example 2 except that the polishing slurry of Example 3 was used instead of the polishing slurry of Example 2.
  • the average polishing rate was as high as 4.7 ⁇ m / hour.
  • the scratches observed before polishing were not confirmed on the sample surface after polishing.
  • the surface roughness was 0.9 nm.
  • Example 4 As the abrasive grains of Example 4, alumina powder having the following physical properties obtained by grinding with a ball mill using aluminum hydroxide produced by the Bayer method as a raw material was used. For the abrasive grains, the number ratio [2] of connected particles having one or more neck portions is evaluated by the above method (1) [Evaluation method 2], and by the above methods (2) to (5). The surface index, the mass average particle diameter, the alkali resistance, and the BET specific surface area were evaluated. The evaluation results are shown below. FIG. 6 shows an SEM image of the abrasive grains of Example 4 in a state where the alumina particles are gathered.
  • polishing slurry of Example 4 was obtained in the same manner as Example 1 except that the polishing abrasive grain of Example 4 was used instead of the polishing abrasive grain of Example 1.
  • polishing Test A polishing test was performed in the same manner as in Example 2 except that the polishing slurry of Example 4 was used instead of the polishing slurry of Example 2.
  • the average polishing rate was as high as 5.3 ⁇ m / hour.
  • the scratches observed before polishing were not confirmed on the sample surface after polishing.
  • the surface roughness was 1.6 nm.
  • Example 5 As the abrasive grains of Example 5, alumina powder having the following physical properties obtained by pulverizing with a jet mill using aluminum hydroxide produced by the Bayer method was used. For the abrasive grains, the number ratio [2] of connected particles having one or more neck portions is evaluated by the above method (1) [Evaluation method 2], and by the above methods (2) to (5). The surface index, the mass average particle diameter, the alkali resistance, and the BET specific surface area were evaluated. The evaluation results are shown below. FIG. 7 shows an SEM image of the abrasive grains of Example 5 in which alumina particles are aggregated.
  • polishing slurry of Example 5 was obtained in the same manner as Example 1 except that the polishing abrasive grain of Example 5 was used instead of the polishing abrasive grain of Example 1.
  • polishing Test A polishing test was conducted in the same manner as in Example 2 except that the polishing slurry of Example 5 was used instead of the polishing slurry of Example 2.
  • the average polishing rate was as high as 5.2 ⁇ m / hour.
  • the scratches observed before polishing were not confirmed on the sample surface after polishing.
  • the surface roughness was 1.0 nm.
  • Comparative Example 1 As the abrasive grains of Comparative Example 1, ⁇ -alumina powder having the following physical properties was used. For the abrasive grains, the number ratio [1] and the number ratio [2] of connected particles having one or more neck portions are evaluated by the above method (1) [Evaluation method 1] and [Evaluation method 2]. The surface index, the mass average particle diameter, the alkali resistance, and the BET specific surface area were evaluated by the above methods (2) to (5). The evaluation results are shown below. FIG. 8 shows an SEM image of the abrasive grains (alpha alumina powder) of Comparative Example 1 in a state where the alumina particles are aggregated.
  • polishing Slurry A polishing slurry of Comparative Example 1 was obtained in the same manner as Example 1, except that the polishing abrasive grain of Comparative Example 1 was used instead of the polishing abrasive grain of Example 1.
  • polishing Test A polishing test was conducted in the same manner as in Example 1 except that the polishing slurry of Comparative Example 1 was used instead of the polishing slurry of Example 1. In Comparative Example 1, the average polishing rate was as low as 3.1 ⁇ m / hour.
  • the polishing slurry containing the abrasive grains of the present invention By using the polishing slurry containing the abrasive grains of the present invention, even a hard brittle material such as sapphire that is difficult to polish, the polishing rate can be increased, and the hard brittleness excellent in surface smoothness. The polishing time for obtaining the material can be shortened. Therefore, industrial utility value is great.

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PCT/JP2016/067994 2015-06-18 2016-06-16 研磨砥粒、研磨スラリーおよび硬脆材の研磨方法、ならびに硬脆材の製造方法 WO2016204248A1 (ja)

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Publication number Priority date Publication date Assignee Title
JP2005001985A (ja) * 2003-05-19 2005-01-06 Sumitomo Chemical Co Ltd 微粒αアルミナの製造法
JP2007055888A (ja) * 2005-07-25 2007-03-08 Sumitomo Chemical Co Ltd 微粒αアルミナ
JP2010515656A (ja) * 2007-01-15 2010-05-13 サン−ゴバン セラミックス アンド プラスティクス，インコーポレイティド セラミック粒状材料及び当該セラミック粒状材料を形成するための方法
WO2011136387A1 (ja) * 2010-04-28 2011-11-03 株式会社バイコウスキージャパン サファイア研磨用スラリー、及びサファイアの研磨方法
WO2012115020A1 (ja) * 2011-02-21 2012-08-30 株式会社 フジミインコーポレーテッド 研磨用組成物
WO2013153618A1 (ja) * 2012-04-10 2013-10-17 住友化学株式会社 アルミナの製造方法

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Publication number Priority date Publication date Assignee Title
JP2005001985A (ja) * 2003-05-19 2005-01-06 Sumitomo Chemical Co Ltd 微粒αアルミナの製造法
JP2007055888A (ja) * 2005-07-25 2007-03-08 Sumitomo Chemical Co Ltd 微粒αアルミナ
JP2010515656A (ja) * 2007-01-15 2010-05-13 サン−ゴバン セラミックス アンド プラスティクス，インコーポレイティド セラミック粒状材料及び当該セラミック粒状材料を形成するための方法
WO2011136387A1 (ja) * 2010-04-28 2011-11-03 株式会社バイコウスキージャパン サファイア研磨用スラリー、及びサファイアの研磨方法
WO2012115020A1 (ja) * 2011-02-21 2012-08-30 株式会社 フジミインコーポレーテッド 研磨用組成物
WO2013153618A1 (ja) * 2012-04-10 2013-10-17 住友化学株式会社 アルミナの製造方法

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