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WO2014122978A1 - Procédé pour la production d'abrasif - Google Patents

Procédé pour la production d'abrasif Download PDF

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Publication number
WO2014122978A1
WO2014122978A1 PCT/JP2014/051041 JP2014051041W WO2014122978A1 WO 2014122978 A1 WO2014122978 A1 WO 2014122978A1 JP 2014051041 W JP2014051041 W JP 2014051041W WO 2014122978 A1 WO2014122978 A1 WO 2014122978A1
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Prior art keywords
core
mol
aqueous solution
shell
precursor
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PCT/JP2014/051041
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English (en)
Japanese (ja)
Inventor
啓介 溝口
奈津紀 伊藤
高橋　篤
智恵 乾
前澤　明弘
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Konica Minolta Inc
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Konica Minolta Inc
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/14—Anti-slip materials; Abrasives
    • C09K3/1436—Composite particles, e.g. coated particles
    • C09K3/1445—Composite particles, e.g. coated particles the coating consisting exclusively of metals
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1204—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material inorganic material, e.g. non-oxide and non-metallic such as sulfides, nitrides based compounds
    • C23C18/1208—Oxides, e.g. ceramics
    • C23C18/1216—Metal oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
    • C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
    • C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
    • C23C18/1229—Composition of the substrate

Definitions

  • the present invention relates to a method for producing an abrasive. More specifically, the present invention relates to a method for producing an abrasive containing core-shell type inorganic particles containing a salt of an element such as yttrium in a core and a salt of an element such as yttrium and a cerium salt in a shell.
  • a rare earth element oxide which is mainly composed of cerium oxide and lanthanum oxide, neodymium oxide, praseodymium oxide, etc.
  • Other abrasives include diamond, iron oxide, aluminum oxide, zirconium oxide, colloidal silica, etc., but when compared in terms of polishing rate and surface roughness of the polished object, cerium oxide Is known to be effective and is used extensively.
  • cerium oxide is unevenly distributed worldwide, and it cannot be said that the supply is stable. Therefore, establishment of a manufacturing method of an abrasive that can perform polishing with high accuracy while reducing the amount of cerium oxide used is required.
  • Patent Document 1 describes a method for obtaining a cerium-based abrasive having a crystallite diameter of 20 to 40 nm (200 to 400 mm) obtained by firing at a temperature of 850 to 1100 ° C. for 1 to 10 hours.
  • a cerium-based abrasive is obtained by mixing and grinding a mixed rare earth oxide and a mixed rare earth fluoride.
  • a glass substrate for hard disk can be mentioned, but in order to increase the recording density, the glass substrate for hard disk can be obtained by reducing the surface roughness of the glass substrate. There is a tendency to shorten the distance to the magnetic head.
  • the glass substrate for hard disk has been increasingly required every year to improve mechanical characteristics, especially hardness and rigidity, in order to suppress disc shake when rotating at high speed.
  • a tempered glass substrate mainly composed of aluminosilicate and a crystallized glass substrate mainly composed of lithium silicate have been used.
  • these glass substrates have excellent chemical resistance and are hard, so the workability is poor, and the polishing rate becomes extremely slower than when polishing a conventional glass substrate. Moreover, since these glass substrates are harder than the conventional glass substrate, there exists a problem that a board
  • An object of the present invention is to provide a method for producing an abrasive capable of reducing the surface roughness of an object to be polished.
  • the present inventor in the process of examining the cause of the above problems, yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium ( Eu), a core containing a salt of at least one element selected from gadolinium (Gd) and terbium (Tb), a salt of at least one element selected from the eight elements, and a salt of cerium (Ce)
  • Y yttrium
  • Ti titanium
  • Ba barium
  • Sm samarium
  • Eu europium
  • a salt of at least one element selected from the eight elements and a salt of cerium (Ce)
  • Ce cerium
  • a method for producing an abrasive containing core-shell type inorganic particles Contains a salt of at least one element selected from yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd) and terbium (Tb) And a precursor of the core-shell type inorganic particles having a shell containing at least one element salt selected from the eight elements and a cerium (Ce) salt within a range of 500 to 1200 ° C.
  • a method for producing an abrasive comprising a firing step of firing within a range of 1 to 5 hours at a temperature.
  • a firing apparatus for firing the precursor in the firing step is a roller hearth kiln or a rotary kiln.
  • the core forming step forms a basic carbonate of at least one element selected from yttrium, titanium, strontium, barium, samarium, europium, gadolinium and terbium by adding a urea compound, Forming a core of the precursor as a main component,
  • an aqueous solution prepared from nitrate of at least one element selected from the eight elements and nitrate of cerium is added, and at least one selected from the eight elements is outside the core.
  • the abrasive according to any one of items 2 to 5, which is a step of forming a shell of the precursor containing an elemental basic carbonate and a cerium basic carbonate. Manufacturing method.
  • the amount of cerium used can be suppressed, a high polishing rate can be obtained for a harder object to be polished, and the surface roughness of the object to be polished can be reduced.
  • the expression mechanism or action mechanism of the effect of the present invention is not clear, but is presumed as follows. By setting the firing temperature in the firing step within the range of 500 to 1200 ° C. and the firing time within the range of 1 to 5 hours, particles having a crystallite size suitable as an abrasive grow and are sufficient for polishing. It is considered that an abrasive containing core-shell type inorganic particles having hardness is obtained.
  • Schematic diagram showing the flow of the abrasive manufacturing process Schematic diagram showing particle crystallites and particle size
  • the graph which shows the temperature change in a temporary baking and a baking process typically Schematic diagram showing the structure of the core-shell type inorganic particles contained in the abrasive
  • the method for producing an abrasive of the present invention is a method for producing an abrasive containing core-shell type inorganic particles, and includes yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium ( Sm), europium (Eu), gadolinium (Gd), a core containing a salt of at least one element selected from terbium (Tb), a salt of at least one element selected from the eight elements, and cerium (Ce)
  • Y yttrium
  • Ti titanium
  • Ba barium
  • Sm samarium
  • Eu europium
  • Gd gadolinium
  • Tb terbium
  • a salt of at least one element selected from the eight elements and cerium (Ce)
  • At least the core / shell type inorganic particle precursor is separated from the reaction solution by at least the core forming step, the shell forming step and the reaction solution.
  • the precursor is produced through a separation step, and the precursor is pre-fired within the range of 300 to 490 ° C. for 1 to 5 hours after the solid-liquid separation step and before the firing step. .
  • an abrasive containing core-shell type inorganic particles having sufficient durability against pressure during polishing is obtained by sufficiently growing crystallites forming the core.
  • the heating rate of the baking temperature in the baking step is in the range of 20 to 50 ° C./min. Thereby, it is thought that the crystallite of the shell containing many cerium salts grows stably.
  • the temperature lowering rate of the temperature for cooling the precursor is within the range of 1 to 20 ° C./min after the firing step. This makes it possible to suppress the generation of minute cracks between the core and the shell, and since the bonding between layers becomes stronger, the core / shell type is resistant to pressure during polishing and has less unevenness on the outermost surface. It is thought that inorganic particles can be formed.
  • the firing apparatus for firing the precursor in the firing step is a roller hearth kiln or a rotary kiln. Thereby, heat is uniformly applied to the precursor of the core / shell type inorganic particles contained in the abrasive, which is preferable.
  • the core forming step forms a basic carbonate of at least one element selected from yttrium, titanium, strontium, barium, samarium, europium, gadolinium and terbium by adding a urea compound
  • ⁇ is used to mean that the numerical values described before and after it are included as a lower limit value and an upper limit value.
  • the method for producing an abrasive of the present invention is a method for producing an abrasive containing core-shell type inorganic particles P, and includes yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), and samarium. (Sm), europium (Eu), gadolinium (Gd), and a core containing at least one element salt selected from terbium (Tb), at least one element salt selected from the eight elements, and cerium (Ce). And a firing step D for firing the precursor of the core-shell type inorganic particles P having a shell containing a salt of 1) at a temperature in the range of 500 to 1200 ° C. for 1 to 5 hours.
  • Typical abrasives include bengara ( ⁇ Fe 2 O 3 ), cerium oxide, aluminum oxide, manganese oxide, zirconium oxide, colloidal silica and other abrasive particles dispersed in water or oil to form a slurry. is there.
  • the present invention is a chemical mechanical polishing method for polishing semiconductor devices and glass, in which polishing is performed by both physical action and chemical action in order to obtain a sufficient polishing rate while maintaining flatness with high accuracy.
  • This is a method for producing an abrasive containing core-shell type inorganic particles P containing cerium capable of being subjected to (CMP; Chemical Mechanical Polishing), and will be described in detail below.
  • polishing material containing the core-shell type inorganic particle P (refer FIG. 4) which consists of the core 1 and the shell 2 is shown.
  • the method for producing core / shell type inorganic particles P (hereinafter also referred to as abrasive particles) of the present invention comprises a core formation step A, a shell formation step B, a solid-liquid separation step C, and a firing step D. It is preferable that it is a manufacturing method of the aspect which consists of these four processes.
  • the core formation step A is at least one selected from yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd), and terbium (Tb).
  • Y yttrium
  • Ti titanium
  • strontium Sr
  • barium Ba
  • Sm samarium
  • Eu europium
  • Gd gadolinium
  • Tb terbium
  • An embodiment is preferable in which a salt of the element is formed, and a core 1 of a precursor of abrasive particles mainly containing the salt is formed.
  • the core 1 may be formed using a salt of at least one element selected from the group consisting of Th and an alkaline earth metal.
  • a yttrium salt and a precipitant are dissolved in water to prepare a solution having a predetermined concentration.
  • the seed crystal of the core 1 is produced by heating and stirring the solution at 80 ° C. or higher.
  • a solution prepared with a yttrium salt is further added to the prepared solution, and the mixture is heated and stirred at 80 ° C. or higher.
  • a solution that has started heating and stirring is referred to as a reaction solution.
  • the salt of at least one element selected from the group consisting of Er, Tm, Yb, Lu, W, Bi, Th and alkaline earth metals, nitrates, hydrochlorides, sulfates, etc. can be used.
  • Nitrate with low impurity contamination for example, yttrium nitrate, titanium nitrate, strontium nitrate, barium nitrate, samarium nitrate, europium nitrate
  • the precipitating agent may be any kind of alkaline compound that produces a basic carbonate when mixed with water with the element salt and heated, and urea compounds, ammonium carbonate, ammonium hydrogen carbonate, and the like are preferable.
  • urea compounds include urea salts (eg, nitrates and hydrochlorides), N, N′-dimethylacetylurea, N, N′-dibenzoylurea, benzenesulfonylurea, p-toluenesulfonylurea, trimethylurea, tetraethylurea , Tetramethylurea, triphenylurea, tetraphenylurea, N-benzoylurea, methylisourea, ethylisourea and the like, and urea is also included.
  • urea compounds urea is particularly preferable in that it gradually hydrolyzes to form a precipitate slowly and a uniform precipitate is obtained.
  • a basic carbonate insoluble in water for example, a basic carbonate of yttrium
  • the deposited precipitate can be dispersed in a monodispersed state.
  • the basic carbonate of cerium is formed also in the shell formation step B described later, a continuous layer structure of the basic carbonate can be formed.
  • the aqueous solution prepared from the salt of yttrium added to the reaction solution in the core formation step A and the shell formation step B is an yttrium nitrate aqueous solution prepared by dissolving yttrium nitrate in water. Show the case. Moreover, although the case where urea is used as a urea compound is shown, it is an example and the present invention is not limited to this.
  • the addition rate of an aqueous solution containing a salt of yttrium is preferably 0.003 mol / L to 5.5 mol / L per minute, and is added to the reaction solution while heating and stirring at 80 ° C. or higher. It is preferable. This is because by setting the addition rate within the above range, spherical abrasive particles having excellent monodispersibility are easily formed. This is because when the heating is performed at 80 ° C. or higher, the added urea is easily decomposed.
  • the urea concentration to be added is preferably 5 to 50 times the yttrium ion concentration.
  • the shell forming step B includes yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd) and terbium (Y) formed by the core forming step A.
  • An embodiment in which the mixed solution is added at a constant rate for a predetermined time is preferable.
  • the shell 2 may be formed using a salt of at least one element selected from the group consisting of alkaline earth metals.
  • cerium salt used for the preparation of the aqueous solution it is preferable to use a nitrate with a small amount of impurities in the product, so the case where cerium nitrate is used has been shown. Sulfates and the like can be used.
  • the addition rate of the aqueous solution added in the shell formation step B is preferably 0.003 mol / L to 5.5 mol / L per minute. This is because by setting the addition rate within the above range, spherical abrasive particles having excellent monodispersibility are easily formed.
  • the concentration ratio of cerium contained in the aqueous solution to be added is preferably 90 mol% or less. This is because when the ratio of the concentration of cerium in the aqueous solution to be added is larger than 90 mol%, when the addition is performed for the same addition time as in the case of adding an aqueous solution prepared to 90 mol% or less, the formed abrasive particles This is because it does not exhibit monodispersibility and may aggregate in a plate shape.
  • the reaction solution is preferably heated and stirred at 80 ° C. or higher while the aqueous solution is added at the addition rate. This is because when heated and stirred at 80 ° C. or higher, decomposition of urea added in the core formation step A easily proceeds.
  • Solid-liquid separation process C In the solid-liquid separation step C, the precursor of the core-shell type inorganic particles P in which the shell 2 is formed in the shell formation step B is separated from the reaction solution. In the solid-liquid separation step C, the precursor of the obtained core / shell type inorganic particles P may be dried and then transferred to the firing step D as necessary.
  • Firing step D In the firing step D, the precursor of the core-shell type inorganic particles P obtained in the solid-liquid separation step C is fired in air or in an oxidizing atmosphere at a temperature of 500 to 1200 ° C. for 1 to 5 hours. To do. Since the precursor of the core-shell type inorganic particle P is calcined to release carbon dioxide, it becomes an oxide from the basic carbonate, and the target core-shell type inorganic particle P is obtained.
  • the crystallite means the maximum region that can be regarded as a single crystal. Specifically, as shown in FIG. 2, one particle is formed of a plurality of crystallites. Since the growth rate of the crystallite changes depending on the firing temperature and time, the core having a crystallite diameter suitable as an abrasive is obtained by firing within a range of 500 to 1200 ° C. for 1 to 5 hours. It is considered that an abrasive containing shell-type inorganic particles P can be produced.
  • a known roller hearth kiln or rotary kiln is preferable. Thereby, heat is uniformly applied to the precursor of the core / shell type inorganic particles P contained in the abrasive, which is preferable.
  • a general roller hearth kiln for example, a plurality of rollers are installed in the furnace, and the raw material is carried on the roller, so that the area in the furnace can be adjusted according to the temperature such as pre-baking, baking, cooling. it can.
  • a general rotary kiln for example, it is substantially cylindrical, and the raw material is gradually fed while slowly rotating in the kiln.
  • the preliminary calcination D ′ is preferably performed within a range of a calcination temperature of 300 to 490 ° C. and a range of 1 to 5 hours.
  • the crystallite forming the core 1 is sufficiently grown, and an abrasive containing the core-shell type inorganic particles P having high durability against the pressure during polishing can be obtained.
  • a known roller hearth kiln or rotary kiln can be used.
  • the temperature in the firing step D is increased at a temperature increase rate within a range of 20 to 50 ° C./min. Thereby, it is considered that the crystallites of the shell 2 containing a large amount of cerium grow stably.
  • the temperature from 500 ° C. to room temperature (25 ° C.) at a temperature lowering rate within the range of 1 to 20 ° C./min.
  • the generation of minute cracks between the core 1 and the shell 2 can be suppressed, and the bonding between the layers becomes stronger, so that the core is resistant to pressure during polishing and has less unevenness on the outermost surface.
  • shell-type inorganic particles P can be formed.
  • FIG. 3 A graph schematically showing the temperature change in the pre-baking D ′ and the baking step D is shown in FIG. 3.
  • the precursor of the core-shell type inorganic particles P is calcined D ′ within the range of 300 to 490 ° C. for 1 to 5 hours before the firing step D, and then 500 to Baking is preferably performed at a temperature in the range of 1200 ° C. for 1 to 5 hours.
  • the firing in the firing step D means firing at a temperature in the range of 500 to 1200 ° C. for 1 to 5 hours.
  • the pre-baking D ′ before the baking step D means pre-baking within the range of 300 to 490 ° C. for 1 to 5 hours before the baking step D.
  • the firing step D may be a temperature change that does not include the holding time for maintaining a constant temperature in the firing time, and the same applies to the temporary firing D ′.
  • the temporary temperature in the following examples is the maximum temperature before the baking step D when there is no temporary baking D ′ or the maximum temperature during temporary baking when there is the temporary baking D ′.
  • the pre-baking time is a time for performing pre-baking within a range of 300 to 490 ° C.
  • the temporary holding time is a time during which the temporary temperature is held in the temporary baking D ′.
  • the temperature is the highest temperature in the firing step D.
  • the firing time is the time for firing in the range of 500 to 1200 ° C. in the firing step D.
  • the holding time is the time during which the maximum temperature is held in the firing step D.
  • the rate of temperature rise represents the rate at which the temperature is raised from 500 ° C. to the maximum temperature in the firing step D.
  • the cooling rate represents a rate of cooling the temperature from 500 ° C. to room temperature (25 ° C.) after the firing step D.
  • the “core-shell type inorganic particles” refers to the core (also referred to as “core portion” or “inner core portion”) constituting the inside including the central portion of the inorganic crystal particles, and the innermost of the inorganic crystal particles.
  • the core may have a structure having a plurality of layers.
  • the structural component of a core and the structural component of a shell may be mixed near a boundary, and a boundary line may be unclear.
  • a boundary line that becomes an interface between the core and the shell is visually confirmed using a transmission electron microscope (TEM).
  • TEM transmission electron microscope
  • the core-shell type inorganic particles P according to the present invention are first sufficiently dispersed in a room temperature curable epoxy resin, then embedded, and dispersed in a styrene fine powder having a particle size of about 100 nm.
  • the core-shell type inorganic particles P according to the present invention preferably have a two-layer structure in which the core 1 including the center and the shell 2 outside the core 1 are provided as shown in FIG.
  • the core 1 is at least one element selected from yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd), and terbium (Tb).
  • Salt for example, yttrium oxide is contained as a main component (60 mol% or more). This is because a salt such as yttrium oxide is less likely to break than cerium oxide against stress applied during polishing.
  • the seed crystal formed in the core formation step A and the basic carbonate formed outside thereof are combined to form the core 1.
  • the core 1 is made of Ce, Al, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Zr, In, Sn, Dy, Ho, Er, Tm, Yb, Lu,
  • a salt of at least one element selected from the group consisting of W, Bi, Th, and alkaline earth metal may be used in combination.
  • the shell 2 is at least one element selected from yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd), and terbium (Tb). Salts such as yttrium oxide and cerium (Ce) salts such as cerium oxide.
  • the shell 2 is at least selected from yttrium (Y), titanium (Ti), strontium (Sr), barium (Ba), samarium (Sm), europium (Eu), gadolinium (Gd), and terbium (Tb).
  • Y yttrium
  • Ti titanium
  • strontium Sr
  • barium Ba
  • Sm samarium
  • Eu europium
  • Gd gadolinium
  • Tb terbium
  • Al, Sc, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Ga, Ge, Zr, In, Sn, Dy, Ho At least one element selected from the group consisting of Er, Tm, Yb, Lu, W, Bi, Th, and alkaline earth metal may be used in combination.
  • the concentration distribution of the shell 2 may be uniform, but a mode in which the composition of cerium oxide continuously increases from the center of the core-shell type inorganic particle P toward the surface is preferable. Specifically, the composition of the portion close to the core 1 on the center side of the core-shell type inorganic particles P in the shell 2 occupies a large proportion of yttrium oxide. Then, as the core-shell type inorganic particles P move from the center side to the surface side, the ratio of the cerium oxide in the composition of the shell 2 continuously increases.
  • region on the outermost surface side may become a fixed ratio.
  • the shape of the core-shell type inorganic particles P is not limited to a spherical shape, and may be a substantially elliptical shape.
  • the particle diameter of the core 1 is preferably in the range of 0.015 to 1.1 ⁇ m. By setting it within this range, it is possible to maintain high durability against pressure applied during polishing.
  • the thickness of the shell 2 is preferably in the range of 0.0025 to 0.45 ⁇ m. By setting this range, core-shell type inorganic particles P exhibiting monodispersity and excellent in polishing rate and durability can be produced.
  • the abrasive particles contained in the abrasive differ in the required level for the particle diameter depending on the use application, but as the finished surface accuracy after polishing becomes higher, the abrasive particles contained in the used abrasive particles become finer. I need it.
  • the average particle size needs to be 2.0 ⁇ m or less for use in the manufacturing process of a semiconductor device.
  • the average particle diameter of the core-shell type inorganic particles P is preferably in the range of 0.02 to 2.0 ⁇ m, and more preferably in the range of 0.05 to 1.5 ⁇ m.
  • an abrasive having the same particle size as possible and having a small particle size distribution variation coefficient.
  • abrasives and deterioration of abrasives Taking a glass substrate as an example, a method of using an abrasive will be described. 1. Preparation of Abrasive Slurry Abrasive powder using the core-shell type inorganic particles P is added to a solvent such as water to prepare an abrasive slurry. By adding a dispersant or the like to the abrasive slurry, aggregation is prevented, and the slurry is constantly stirred using a stirrer or the like to maintain a dispersed state. The abrasive slurry is circulated and supplied to the polishing machine using a supply pump.
  • polishing process The glass substrate is brought into contact with the upper and lower surface plates of the polishing machine to which the polishing pad (polishing cloth) is applied, and the pad and the glass are moved relative to each other under pressure while supplying the abrasive slurry to the contact surface. It is polished by that.
  • the abrasive material is used under pressure as in the polishing step. For this reason, the core-shell type inorganic particles P contained in the abrasive gradually collapse and become finer as the polishing time elapses. Since miniaturization of the core-shell type inorganic particles P causes a reduction in the polishing rate, the core-shell type inorganic particles P having a small change in particle size distribution before and after polishing are desired.
  • the firing in the firing step D means firing at a temperature in the range of 500 to 1200 ° C. for 1 to 5 hours.
  • the pre-baking D ′ before the baking step D means pre-baking within the range of 300 to 490 ° C. for 1 to 5 hours before the baking step D.
  • the temporary temperature in the table is the maximum temperature in the temporary baking D ′.
  • the pre-baking time is the time for performing pre-baking D ′ within the range of 300 to 490 ° C.
  • the temporary holding time is a time during which the temporary temperature is held in the temporary baking D ′.
  • the temperature is the highest temperature in the firing step D.
  • the firing time is the time for firing in the range of 500 to 1200 ° C. in the firing step D.
  • the holding time is the time during which the maximum temperature is held in the firing step D.
  • the rate of temperature rise represents the rate at which the temperature is raised from 500 ° C. to the maximum temperature in the firing step D.
  • the temperature decreasing rate represents a rate of cooling the temperature from 500 ° C. to room temperature (25 ° C.) after the firing step D.
  • Example 1 ⁇ Abrasive Material 1: Examples> (1) Prepare 2 L of 0.02 mol / L yttrium nitrate (III) aqueous solution (hereinafter, simply referred to as “yttrium nitrate aqueous solution”), and then mix it with this aqueous solution so that urea is 0.60 mol / L. The seed crystal was produced by heating and stirring at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 2 Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 3 Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 4 Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 5 Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 8 Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 9 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 10 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 11 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive 12 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 13 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive 14 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive 15 Comparative Example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive material 16 Comparative example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive material 17 Comparative example> (1) 2 L of a 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. to prepare a seed crystal. . (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • polishing speed The polishing machine used for polishing processing is to be polished while supplying abrasive slurry in which abrasive powder using core-shell type inorganic particles P is dispersed in a solvent such as water to the surface to be polished.
  • the surface is polished with a polishing cloth.
  • the abrasive slurry was water only as a dispersion medium, and the concentration was 100 g / L.
  • polishing was performed by circulatingly supplying an abrasive slurry at a flow rate of 5 L / min.
  • a glass substrate made of crystallized glass of 65 mm ⁇ was used as an object to be polished, and a polyurethane cloth was used as the polishing cloth.
  • the polishing pressure on the polished surface was 9.8 kPa (100 g / cm 2 ), the rotation speed of the polishing tester was set to 100 min ⁇ 1 (rpm), and polishing was performed for 30 minutes.
  • the thickness before and after polishing was measured with Nikon Digimicro (MF501), and the polishing amount per minute ( ⁇ m) was calculated from the thickness displacement, and was used as the polishing rate.
  • Polishing speed ⁇ Faster than 1.0 ⁇ m / min ⁇ : Within the range of 0.3 to 1.0 ⁇ m / min ⁇ : Less than 0.3 ⁇ m / min Surface condition ⁇ : Surface roughness Ra is less than 0.15 ⁇ m ⁇ : Surface Roughness Ra is in the range of 0.15 ⁇ m or more and less than 0.3 ⁇ m ⁇ : Surface roughness Ra is in the range of 0.3 to 0.5 ⁇ m ⁇ : Surface roughness Ra is rougher than 0.5 ⁇ m
  • the abrasives 1 to 8 as examples of the present invention had a surface roughness Ra as the surface condition of the object to be polished within a polishing rate of 0.3 to 1.0 ⁇ m / min. 0.5 ⁇ m or less. Therefore, it has been found that it is excellent in production as an abrasive and is suitable for using an object to be polished as a hard disk device (HDD).
  • HDD hard disk device
  • the polishing materials 9 to 17 as comparative examples had a polishing rate of less than 0.3 ⁇ m / min, and the result was that the surface roughness Ra was rougher than 0.5 ⁇ m as the surface state of the object to be polished.
  • the baking temperature in the baking step D was in the range of 500 to 1200 ° C., and the baking rate in the example in which the baking time was in the range of 1 to 5 hours was higher than that of the comparative example. It was found that the surface condition was good.
  • Example 2 ⁇ Abrasive 18: Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 19 Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 21 Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive Material 23 Comparative Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • the abrasives 19 to 22 which are examples of the present invention have a surface roughness Ra of less than 0.15 ⁇ m, and are better than the abrasives 4 and 18, which are less susceptible to scratches. It turned out to be an abrasive. This is because by performing preliminary firing at 300 to 490 ° C., crystallites forming the core 1 are sufficiently grown, and core-shell type inorganic particles P having high durability against pressure during polishing are obtained. It is considered that good results were obtained.
  • the abrasive 23 as a comparative example was temporarily fired at 300 ° C. for 1 hour, but because the firing temperature in the firing step D was 450 ° C., the core-shell type inorganic particles P did not grow sufficiently, It is considered that a sufficient polishing rate and surface condition as an abrasive were not obtained.
  • Example 3 ⁇ Abrasive Material 24: Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • Example> 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • the abrasives 24 and 25, which are examples of the present invention, are abrasives having a polishing rate faster than 1.0 ⁇ m / min and superior to the abrasive 4 in terms of production efficiency. It was found to be a better abrasive that can reduce the amount of abrasive used because it is high. This is because when the temperature increase rate in the firing step D is set to 20 to 50 ° C./min, the crystallites of the shell 2 containing a large amount of cerium grow stably, so that an excellent abrasive with a higher polishing rate can be obtained. It is thought that it was obtained.
  • Example 4 ⁇ Abrasive Material 26: Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • ⁇ Abrasive material 27 Example> (1) 2 L of 0.02 mol / L yttrium nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, and heated and stirred at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of yttrium nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. A core 1 made of salt was formed.
  • the abrasives 26 and 27 according to the examples of the present invention are abrasives having a surface state superior to that of the abrasive 24. This can suppress the occurrence of minute cracks between the core 1 and the shell 2 by setting the temperature drop rate during cooling after the firing step D within the range of 1 to 20 ° C./min. It is considered that an abrasive containing the core-shell type inorganic particles P that is strong against the pressure during polishing and has few irregularities on the outermost surface is obtained because the bonding between the layers becomes stronger.
  • Example 5 ⁇ Abrasive 28: Example> (1) 2 L of a 0.02 mol / L titanium nitrate (IV) aqueous solution was prepared, and then mixed with the aqueous solution so that urea was 0.60 mol / L, followed by heating and stirring at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of titanium nitrate (IV) having a concentration of 1.6 mol / L was added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. Core 1 consisting of basic carbonate was formed.
  • Example> 2 L of a 0.02 mol / L strontium (II) nitrate aqueous solution was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, followed by heating and stirring at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of strontium nitrate (II) having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C., Core 1 consisting of basic carbonate was formed.
  • ⁇ Abrasive material 32 Example> (1) A 0.02 mol / L aqueous solution of europium (III) nitrate (2 L) was prepared, and then mixed with this aqueous solution so that urea was 0.60 mol / L, followed by heating and stirring at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of europium (III) nitrate having a concentration of 1.6 mol / L is added with heating and stirring at 90 ° C. for 65 minutes at an addition rate of 1 mL / min, Core 1 consisting of basic carbonate was formed.
  • ⁇ Abrasive material 33 Example> (1) A 2 L aqueous solution of 0.02 mol / L gadolinium (III) nitrate was prepared, and then mixed with the aqueous solution so that urea was 0.60 mol / L, followed by heating and stirring at 90 ° C. (2) To the reaction solution obtained in (1) above, an aqueous solution of gadolinium (III) nitrate having a concentration of 1.6 mol / L is added at a rate of 1 mL / min for 65 minutes with heating and stirring at 90 ° C. Core 1 consisting of basic carbonate was formed.
  • the abrasives 28 to 34 according to the examples of the present invention were found to be excellent abrasives as the abrasive 4 was. This is because the elements used in the abrasives 28 to 34 are resistant to the high pressure applied to the core 1 during polishing, like yttrium, and the shell 2 is contained together with cerium so that it is contained in the shell and between the core and shell. This is thought to be due to the increased binding power.
  • the present invention may be used in the field of polishing with an abrasive containing cerium oxide in the manufacturing process of glass products, semiconductor devices, crystal oscillators and the like.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Ceramic Engineering (AREA)
  • Composite Materials (AREA)
  • Finish Polishing, Edge Sharpening, And Grinding By Specific Grinding Devices (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

L'invention a pour objet un procédé pour la production d'un abrasif qui réduit au minimum la quantité d'oxyde de cérium utilisé, qui permet d'obtenir une vitesse de polissage élevée pour un objet devant être poli ayant une plus grande dureté et qui permet de réduire la rugosité de surface de l'objet devant être poli. Ce procédé pour la production d'un abrasif utilise des particules inorganiques à structure cœur-coquille (P) et il est caractérisé en ce qu'il comprend une étape de cuisson (D) pour la cuisson, pendant une à cinq heures à une température comprise dans la plage de 500-1200°C, d'un précurseur des particules inorganiques à structure cœur-coquille (P) comprenant : un cœur contenant un sel d'au moins un élément choisi parmi l'yttrium (Y), le titane (Ti), le strontium (Sr), le baryum (Ba), le samarium (Sm), l'europium (Eu), le gadolinium (Gd) et le terbium (Tb) ; et une coquille (2) contenant un sel d'au moins un élément choisi parmi les huit éléments ci-dessus et un sel de cérium (Ce).
PCT/JP2014/051041 2013-02-05 2014-01-21 Procédé pour la production d'abrasif Ceased WO2014122978A1 (fr)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356312A (ja) * 2001-03-24 2002-12-13 Degussa Ag コア、ドーピング成分およびシェルを有する酸化物粒子、その製法およびその使用
WO2004009726A1 (fr) * 2002-07-19 2004-01-29 Saint-Gobain Ceramics & Plastics, Inc. Particules abrasives a revetement de sel de cerium pour le polissage de verre
WO2005035688A1 (fr) * 2003-10-10 2005-04-21 Korea Institute Of Ceramic Engineering & Technology Abrasif pour le polissage chimique mecanique et procede de production associe
WO2006049197A1 (fr) * 2004-11-08 2006-05-11 Asahi Glass Company, Limited PROCÉDÉ SERVANT À PRODUIRE DE FINES PARTICULES DE CeO2 ET SUSPENSION ÉPAISSE DE POLISSAGE CONTENANT DE TELLES FINES PARTICULES
WO2008044685A1 (fr) * 2006-10-10 2008-04-17 National Institute Of Advanced Industrial Science And Technology Microparticule d'oxyde de cérium de type noyau-coquille, solution de dispersion comprenant la microparticule et procédé de production de la microparticule ou de la solution de dispersion
JP2008182179A (ja) * 2006-12-27 2008-08-07 Hitachi Chem Co Ltd 研磨剤用添加剤、研磨剤、基板の研磨方法及び電子部品
WO2010139603A1 (fr) * 2009-06-05 2010-12-09 Basf Se Nanostructures d'oxyde de métal de type framboise enrobées avec des nanoparticules de ceo2 pour la planarisation chimique-mécanique (cmp)
JP2012011526A (ja) * 2010-07-02 2012-01-19 Admatechs Co Ltd 研磨材およびその製造方法
WO2012101871A1 (fr) * 2011-01-25 2012-08-02 コニカミノルタホールディングス株式会社 Particules abrasives fines et processus pour leur production
WO2014038536A1 (fr) * 2012-09-05 2014-03-13 コニカミノルタ株式会社 Procédé de production de particules de matériau de polissage

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2002356312A (ja) * 2001-03-24 2002-12-13 Degussa Ag コア、ドーピング成分およびシェルを有する酸化物粒子、その製法およびその使用
WO2004009726A1 (fr) * 2002-07-19 2004-01-29 Saint-Gobain Ceramics & Plastics, Inc. Particules abrasives a revetement de sel de cerium pour le polissage de verre
WO2005035688A1 (fr) * 2003-10-10 2005-04-21 Korea Institute Of Ceramic Engineering & Technology Abrasif pour le polissage chimique mecanique et procede de production associe
WO2006049197A1 (fr) * 2004-11-08 2006-05-11 Asahi Glass Company, Limited PROCÉDÉ SERVANT À PRODUIRE DE FINES PARTICULES DE CeO2 ET SUSPENSION ÉPAISSE DE POLISSAGE CONTENANT DE TELLES FINES PARTICULES
WO2008044685A1 (fr) * 2006-10-10 2008-04-17 National Institute Of Advanced Industrial Science And Technology Microparticule d'oxyde de cérium de type noyau-coquille, solution de dispersion comprenant la microparticule et procédé de production de la microparticule ou de la solution de dispersion
JP2008182179A (ja) * 2006-12-27 2008-08-07 Hitachi Chem Co Ltd 研磨剤用添加剤、研磨剤、基板の研磨方法及び電子部品
WO2010139603A1 (fr) * 2009-06-05 2010-12-09 Basf Se Nanostructures d'oxyde de métal de type framboise enrobées avec des nanoparticules de ceo2 pour la planarisation chimique-mécanique (cmp)
JP2012011526A (ja) * 2010-07-02 2012-01-19 Admatechs Co Ltd 研磨材およびその製造方法
WO2012101871A1 (fr) * 2011-01-25 2012-08-02 コニカミノルタホールディングス株式会社 Particules abrasives fines et processus pour leur production
WO2014038536A1 (fr) * 2012-09-05 2014-03-13 コニカミノルタ株式会社 Procédé de production de particules de matériau de polissage

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