US20060058426A1 - Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition - Google Patents

Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition Download PDF

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Publication number
US20060058426A1
US20060058426A1 US11/220,402 US22040205A US2006058426A1 US 20060058426 A1 US20060058426 A1 US 20060058426A1 US 22040205 A US22040205 A US 22040205A US 2006058426 A1 US2006058426 A1 US 2006058426A1
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Prior art keywords
alumina particle
resin composition
manufacturing
temperature
alumina
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Inventor
Takashi Oda
Yasuaki Kai
Tomohiro Itou
Takashi Seino
Hironobu Muramatsu
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Nissan Motor Co Ltd
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Nissan Motor Co Ltd
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Assigned to NISSAN MOTOR CO., LTD. reassignment NISSAN MOTOR CO., LTD. ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MURAMATSU, HIRONOBU, ITOU, TOMOHIRO, KAI, YASUAKI, ODA, TAKASHI, SEINO, TAKASHI
Publication of US20060058426A1 publication Critical patent/US20060058426A1/en
Priority to US13/469,302 priority Critical patent/US8722765B2/en
Abandoned legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/021—After-treatment of oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00—Use of pretreated ingredients
    • C08K9/04—Ingredients treated with organic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
    • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
    • C09C1/40—Compounds of aluminium
    • C09C1/407—Aluminium oxides or hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/54—Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability

Definitions

  • the present invention relates to an alumina particle composite, a method of manufacturing the alumina particle composite, a resin composition and a method of manufacturing the resin composition.
  • Transparent resin applicable as an alternative of inorganic glass includes acrylic resin, polycarbonate resin, polyester resin, styrene resin, epoxy resin, and the like.
  • the resin glass has a feature in being excellent in impact resistance, lightweight properties, and moldability as compared with the inorganic glass.
  • problems concerning a linear expansion coefficient, rigidity, strength, flame retardancy are inherent in the resin glass under the current technology, and the resin glass cannot meet performance required for the automotive parts from a viewpoint of passenger protection. Therefore, under the current situation, such a transparent resin material for use in an automobile is limited to application to a small part such as a cover for an automotive lamp represented by a headlamp.
  • organic/inorganic nanocomposite materials In order to make transparency of the resin and an improvement of mechanical strength thereof compatible with each other, a research on organic/inorganic nanocomposite materials becomes one of solving measures therefor.
  • Representative ones of the research on the organic/inorganic nanocomposite materials include: “Composite Material and Manufacturing Method Thereof” (Japanese Patent No. 2519045) by Toyota Central R&D Labs., Inc.; “Polyamide Composite Material and Manufacturing Method Thereof” (Japanese Patent Examined Publication No. H07-47644 (published in 1995)) by Ube Industries, Ltd. and others; “Polyolefin Composite Material and Manufacturing Method Thereof” (Japanese Patent Unexamined Publication No. H10-30039 (published in 1998)) by Showa Denko K.K.; and the like.
  • dispersion of the filler in the resin accounts for a large factor on maintaining the transparency of the resin and improving the properties thereof.
  • many various dispersion methods in which selection of microparticles, surface treatment of the particles and optimization of composite synthesis are combined are disclosed.
  • Japanese Patent Examined Publication No. H07-47644 discloses a method of immersing caprolactam as a material of nylon between layers of montmorillonite and polymerizing the caprolactam therewith, thereby obtaining a composite of the nylon and the filler.
  • the transparent resin composition obtained by the method of Japanese Patent Unexamined Publication No. H11-343349 can improve various properties such as the strength, the elastic modulus and the impact resistance in a state of maintaining the transparency to some extent.
  • an aspect ratio of a silica particle is 1, the various properties described above except the transparency cannot be improved sufficiently, resulting in that it has been impossible to put the transparent resin composition into practical use for the automotive parts.
  • the present invention has been created in order to solve the above-described problems. It is an object of the present invention to provide filler improving strength, elastic modulus and impact resistance of resin, and to provide a resin composition having higher transparency, which is excellent in strength, elastic modulus and impact resistance.
  • the first aspect of the present invention provides an alumina particle composite comprising: an alumina particle; and an organic acid chemically bonded to a surface of the alumina particle.
  • the second aspect of the present invention provides a method of manufacturing an alumina particle composite comprising: adding an alkali aqueous solution in an aqueous solution with an aluminum salt to produce a reaction mixture containing a gel material of aluminum hydroxide; first heating the reaction mixture at a first temperature not lower than room temperature; after the first heating, second heating the reaction mixture at a second temperature higher than the first temperature; after the second heating, third heating the reaction mixture at a third temperature lower than the second temperature; and after the third heating, fourth heating the reaction mixture at a fourth temperature not less than the room temperature; and dispersing boehmite particles generated in the reaction mixture into a solvent, and adding an organic acid to the solvent.
  • the third aspect of the present invention provides a resin composition comprising: resin; and an alumina particle composite contained in the resin as a filler, the alumina particle composite comprising: an alumina particle; and an organic acid chemically bonded to a surface of the alumina particle.
  • the fourth aspect of the present invention provides a method of manufacturing a resin composition
  • a method of manufacturing the alumina particle composite comprises: adding an alkali aqueous solution in an aqueous solution with an aluminum salt to produce a reaction mixture containing a gel material of aluminum hydroxide; first heating the reaction mixture at a first temperature not lower than room temperature; after the first heating, second heating the reaction mixture at a second temperature higher than the first temperature; after the second heating, third heating the reaction mixture at a third temperature lower than the second temperature; and after the third heating, fourth heating the reaction mixture at a fourth temperature not less than the room temperature; and dispersing boehmite particles generated in the reaction mixture into a second
  • FIG. 1 is a schematic view of an alumina particle composite of the present invention
  • FIG. 2 is a schematic view for explaining a long axis and a short axis
  • FIG. 3 is an electron microscope photograph of a boehmite particle composite manufactured by Example 1;
  • FIG. 4 is an electron microscope photograph of a cross section of the boehmite particle composite manufactured by Example 1;
  • FIG. 5 is an electron microscope photograph of a dispersion liquid of boehmite particles manufactured by Example 1;
  • FIG. 6 is an electron microscope photograph of a dispersion liquid of boehmite particles manufactured by Example 2;
  • FIG. 7 is an exterior photograph of a transparent resin piece obtained by Example 5.
  • FIG. 8 is a table showing experiment conditions and evaluation results of resin compositions of Examples.
  • FIG. 9 is a table showing experiment conditions and evaluation results of resin compositions of Comparative examples.
  • An alumina particle composite as filler of the present invention contains an organic acid chemically bonded to alumina particles.
  • an organic acid 3 is provided on a surface of an alumina particle 2 , and alumina present on a surface layer of the alumina particle 2 and the organic acid 3 are chemically bonded to each other.
  • the organic acid 3 As the organic acid 3 , usable is a compound containing a sulfonic acid group, a carboxyl group or a hydroxyl group, or a compound having a structure belonging to those of boric acids, phosphoric acids or amino acids. Among them, preferable is the compound containing the sulfonic acid group, which can be strongly bonded to the alumina particles, or the organic acid containing the phosphoric acid or the boric acid which is rich in type and favorably available from the market.
  • an inorganic acid is also usable; however, hydrochloric acid, sulfuric acid, nitric acid and the like, each of which has a strong acidity, break a crystalline structure of the particles, and dissolve surfaces of the alumina particles, thereby changing a form of the alumina particles when concentrations thereof are high. Accordingly, it is difficult to adjust the concentrations.
  • Each of inorganic phosphoric acid and carbonic acid has a weak acidity, and bonding power thereof to the alumina particles becomes insufficient.
  • the organic acids are preferable, and among them, the organic acid containing the sulfonic acid group is more preferable.
  • organic acids may be used singly or in combination of two or more thereof.
  • Alkylbenzene sulfonic acid and a sulfonic acid compound to be described below are preferable as the compound containing the sulfonic acid group, however, the compound is not limited to these.
  • boric acids usable in the present invention are methylboric acid, phenylboric acid, butylboric acid, isopropylboric acid, 4-chlorophenylboric acid, 4-hydroxyphenylboric acid, 1,4-phenylenebisboric acid, 4-carboxylphenylboric acid, and the like.
  • the boric acids are not limited to these.
  • a mode of chemical bonding of the organic acid 3 to the alumina particle 2 is a covalent bond, a coordinate bond, a hydrogen bond, an electrostatic bond, and the like.
  • a content of the organic acid in the alumina particle composite is not particularly limited as long as a light transmittance of a dispersion liquid of the alumina particles, which is to be used in a polymerization process of a resin composition to be described later, is 40% or more.
  • a blended amount of the organic acid with 1 mol of the alumina particles is preferably 1 mmol or more, more preferably, 10 mmol or more. If the blended amount of the organic acid is less than 1 mmol, it is impossible to obtain a dispersion liquid of the alumina particles in which the alumina particles are dispersed uniformly in an organic solvent.
  • the blended amount of the organic acid can be measured by combining apparatuses for a TG-DTA, an IR, an NMR and the like.
  • the number of moles of the alumina particles is obtained by a general formula.
  • molecular weights of a alumina particles and y alumina particles are defined as 101.96 by a general formula Al 2 O 3 .
  • a molecular formula AlO(OH) is applied to a calculation of a molecular weight thereof, and the molecular weight is defined as 59.98.
  • the alumina particles 2 be represented by the following General Formula (I). Al 2 O 3 .nH 2 O Formula I
  • the formula represents an aluminum oxide, which is ⁇ and ⁇ alumina, or ⁇ , ⁇ , ⁇ , ⁇ , ⁇ , ⁇ ′, ⁇ , ⁇ , ⁇ and ⁇ alumina.
  • the formula represents boehmite.
  • the formula represents a mixture of boehmite and alumina hydrate with an amorphous structure. This is generally referred to as pseudo boehmite.
  • the formula represents alumina hydrate with an amorphous structure.
  • the alumina particles as the filler is characterized in being at least one selected from these.
  • the alumina particles preferable as the filler for the resin composition are a alumina, ⁇ alumina and boehmite in terms of stability and easiness in manufacturing.
  • a shape of the alumina particles may be any of fiber-like, spindle-like, stick-like, needle-like, tubular and columnar.
  • a length of a short axis be within a range from 1 to 10 nm
  • a length of a long axis be within a range from 20 to 400 nm
  • an aspect ratio be within a range from 5 to 80.
  • the particles be needle-like crystals with the length of the short axis being 6 nm or less.
  • the long axis indicates a long side a of the rectangle A
  • the short axis indicates a short side b of the above smallest rectangle A.
  • the aspect ratio indicates a value of the long axis length/the short axis length (a/b).
  • each alumina particle 2 includes a cylindrical hollow 4 therein.
  • the diameter thereof is within a range from 0.5 to 9.5 nm according to the short axis length of the particles 2 , and the length thereof is within a range from 5 to 400 nm, which is not more than the long axis length of the particles.
  • This can reduce the specific gravity of the alumina particles 2 . Accordingly, when the alumina particles 2 are contained as the filler in the resin, while the weight of the obtained resin composition is being maintained at a comparatively lightweight, the mechanical strength of the obtained resin composition can be increased, and the high transparency thereof can be achieved.
  • the hollow 4 inside is not an essential element. In other words, the alumina particles 2 can achieve the object of the present invention without the hollow 4 .
  • an alkaline aqueous solution is added to an aluminum salt aqueous solution to prepare a gel material of aluminum hydroxide.
  • the aluminum salt constituting the aluminum salt aqueous solution is at least an aluminum salt selected from aluminum chloride anhydride, aluminum chloride hexahydrate, aluminum bromide, aluminum bromide hexahydrate, aluminum iodide, aluminum nitrate nonahydrate, aluminum lactate, aluminum sodium sulfate dodecahydrate (sodium alum), aluminum perchlorate nonahydrate, aluminum isopropoxide, aluminum s-butoxide, aluminum t-butoxide, and the like.
  • aluminum chloride hexahydrate, aluminum nitrate nonahydrate, aluminum bromide hexahydrate, aluminum sodium sulfate dodecahydrate, and aluminum isopropoxide are preferred, which are easily available on the market, easy to use, and cheap.
  • the alkaline aqueous solution is added to an action system to promote hydrolysis of the aluminum salt.
  • An alkaline compound constituting the alkaline aqueous solution can be at least one selected from sodium hydroxide, potassium hydroxide, calcium hydroxide, barium hydroxide, and the like. Sodium hydroxide is particularly preferred.
  • an amount of the alkaline compound is two to four times the amount of aluminum salt in molar ratio.
  • a ratio of a concentration of the aqueous solution with the aluminum salt and a concentration of the alkali aqueous solution is 1 ⁇ 4 to 1 ⁇ 2 in molar ratio.
  • the alkaline compound less than two times is insufficient to produce a reaction product by performing a heat treatment.
  • gelation of the reaction solution is not caused, and the particles cannot be obtained with a good yield.
  • the amount of the alkaline compound is more than four times that of the aluminum salt, the pH of the reaction mixture is too high, and the alkali dissolves the gel, thus increasing adhering and aggregating particles in some cases.
  • the concentration of the aluminum salt aqueous solution is within a range from 0.1 to 0.3 M, and the concentration of the alkaline aqueous solution is within a range from 4.0 to 10.0 M. This can facilitate formation of the gel material in the reaction mixture of the aluminum salt aqueous solution and the alkaline aqueous solution.
  • the concentration of the metallic salt in the aluminum salt aqueous solution is, as described above, preferably, 1.0 to 3.0 M and is more preferably 3.0 M in terms of the productivity.
  • the form of the desired boehmite particles can be controlled by changing the pH of the reaction mixture.
  • the closer the pH is to 4 the longer the long axis of the aluminum particles 1 is, and the higher the aspect ratio thereof is.
  • the closer the pH is to 9 the shorter the long axis of the aluminum particles 1 is, and the lower the aspect ratio thereof is.
  • the pH is less than 4 or more than 9, plate-shaped particles or amorphous particles increase in some cases.
  • the pH value of the reaction mixture can be controlled by changing the concentration and the volume of the alkaline aqueous solution.
  • the volume of the aluminum salt aqueous solution is equal to or larger than the alkaline aqueous solution.
  • concentration of the alkaline aqueous solution is low and the volume thereof is too much, the gelation is less likely to occur.
  • concentration of the aluminum salt aqueous solution and the volumes of the aluminum salt aqueous solution and alkali aqueous solution are fixed, the form of the particles can be controlled by only changing the concentration of the alkali aqueous solution. Accordingly, setting the volumes same is more preferable for reducing the number of items of the synthesis condition.
  • the gel material can be formed in the reaction mixture.
  • the boehmite particles in the growth process are stabilized in the gel material, and adherence and aggregation of the particles are suppressed. It is therefore possible to obtain nano-sized boehmite particles with the particle size distribution range narrowed.
  • first to fourth heat treatments are sequentially carried out.
  • the following heat treatments are carried out while the boehmite particles in the growth process are fixed in the gel material. Accordingly, the particle size distribution range can be extremely narrowed, or the standard deviation can be reduced. As described below, the particle size distribution range can be widened to some extent by properly changing conditions of the heat treatments.
  • the first heat treatment is carried out by heating the reaction mixture to a first temperature not less than the room temperature.
  • the first heat treatment is mainly to promote hydrolysis of the alkali metal salt generated in the reaction mixture and promote formation of the gel material in the reaction mixture.
  • the first temperature may be within a range from a room temperature (25° C.) to 140° C., and preferably, 120 to 140° C. considering reaction time. If the first heat treatment is carried out at a temperature above 140° C., boehmite particles with different lengths are generated, and in some cases, the particle size distribution range of the boehmite particles cannot be narrowed even after the subsequent heat treatments are carried out.
  • the heat treatment time is 24 hours or more. In the case of less than 24 hours, the standard deviation of the particle size is difficult to reduce.
  • the second heat treatment is carried out.
  • the reaction mixture is heated to a second temperature higher than the first temperature of the first heat treatment.
  • the second heat treatment is carried out mainly to obtain boehmite particles with a high aspect ratio.
  • the second temperature needs to be higher than the first temperature and is specifically within a range from 140 to 250° C. In particular, 170 to 250° C. is preferred.
  • the temperature is lower than 140° C., it takes a long time to generate the particles, and as well as the particle size distribution range is widened.
  • temperature higher than 250° C. is advantageous in manufacturing particles with a small aspect ratio.
  • temperature higher than 250° C. is not recommended in this manufacturing method because the heat and pressure resistances of an autoclave of a normal grade on the market have upper limits at 250° C. and a great amount of energy is required when the temperature is higher than 250° C.
  • the heat treatment time in the second heat treatment is preferably within a range from 10 to 30 minutes containing a temperature increasing step, and varies depending on the second temperature. Heating for more than the above time considerably increases the standard deviation of the average particle diameter and turns the needle-shaped particles and the plate-shaped particles into a spindle shape and a particle shape, respectively, reducing the aspect ratio.
  • the third heat treatment is carried out.
  • This third heat treatment is carried out at a third temperature lower than the second temperature in the second heat treatment.
  • the third heat treatment is performed mainly to narrow the particle size distribution range of the boehmite particles.
  • the third temperature is set to, for example, 130° C. or lower and preferably, set to the room temperature or lower. It is preferable that the reaction mixture is set to the third temperature by rapid cooling from the second temperature in the second heat treatment. In this case, considering a cost of a cooler and resistance of a vessel to temperature variation, the third heat treatment can be performed by putting the vessel for the heat treatments into running water. Preferably, the time required for the cooling is shorter. Specifically, it is preferable that the time required for cooling is within 10 minutes. The third heat treatment time is preferably 10 minutes or more containing the time required for cooling. This can narrow the particle size distribution range of the desired boehmite particles.
  • This fourth heat treatment is performed mainly to grow the boehmite particles with a high aspect ratio.
  • a fourth temperature of the fourth heat treatment needs to be set within a temperature range from 100 to 180° C. If the fourth temperature is higher than 180° C., the particle size distribution range increases, and the standard deviation increases. Moreover, needle-shaped and plate-shaped particles are turned into spindle and particle shapes, respectively, thus reducing the aspect ratio in some cases.
  • the fourth heat treatment if the heat treatment is performed at a temperature of 180° C. or more, the produced particles are remelted and recrystallized (Ostwald ripening), and the shape of the particles and the particle size distribution range cannot be controlled in some cases, which sometimes increases the particle size distribution range.
  • the fourth temperature is lower than 100° C., the yield is reduced in some cases.
  • the treatment time is four hours to one week, and heating time varies depending on a temperature setting.
  • boehmite particles with a short axis length of 1 to 10 nm, a long axis length of 20 to 400 nm, and an aspect ratio of 50 to 80. Moreover, the standard deviations of the size property values can be suppressed within 10%. Accordingly, when the resin composition is manufactured by causing the boehmite particles to be contained in the predetermined resin, variation in the properties thereof can be reduced. It is therefore possible to produce goods with stable quality from the resin composition.
  • boehmite particles with different sizes can be manufactured. This can be achieved by carrying out the first heat treatment at a temperature of 140° C. or more for three hours or more and omitting the second to fourth heat treatments. In this case, the standard deviations of the size property values can be 20% or more.
  • the obtained boehmite particles are subjected to a baking treatment.
  • the baking treatment is performed, for example, at 450 to 1500° C. for 1 to 3 hours.
  • the boehmite particles obtained by the aforementioned method is put into an alumina crucible and then heated at 1000° C. for 4 hours, thus obtaining a alumina particles.
  • the temperature increase and decrease rates are 2° C./min.
  • the boehmite particles serving as a raw material by taking means such as freeze drying the boehmite dispersed into water, or spray drying the same.
  • the boehmite particles are dried in a heat oven or naturally dried, the particles are strongly fixed to one another, and the a alumina particles obtained later becomes incapable of being redispersed into the organic solvent or water.
  • the alumina particle composite 1 is made of the alumina particles 2 obtained as described above, and subsequently, a dispersion liquid is prepared, in which the alumina particle composite is dispersed into the organic solvent or water.
  • a method of dispersing the alumina particle composite into the organic solvent is described.
  • the alumina particles obtained as described above are forcibly dispersed into the organic solvent by using at least one means of an ultrasonic wave, a microbead mill, stirring, and high-pressure emulsion, and subsequently, the organic acid containing the predetermined sulfonic acid group, carboxyl group or hydroxyl group, or the boric acid, the phosphoric acid or the amino acid is added thereto.
  • the target alumina particle composite can be obtained, and simultaneously, the dispersion liquid in which the alumina particles are dispersed into the organic solvent can be obtained.
  • the organic acid for use is not dissolved into the organic solvent and does not react with the alumina particles. Accordingly, in this case, it is necessary to disperse the alumina particles into water once.
  • the means such as the ultrasonic wave, the microbead mill, the stirring, and the high-pressure emulsion is used.
  • the organic acid salt is added to the obtained mixed liquid of water and the alumina, the target alumina particle composite can be obtained. Then, solvent exchange is performed from water to the organic solvent by performing centrifugal separation, distillation, and so on, thus making it possible to obtain the dispersion liquid.
  • the dispersion of the boehmite particles by the ultrasonic wave is performed by putting the boehmite particles and water into a predetermined ultrasonic dispersion apparatus and driving the apparatus concerned according to a usual procedure.
  • the dispersion of the boehmite particles by the microbead mill is performed by putting the boehmite particles and water into a predetermined microbead mill dispersion apparatus and driving the apparatus concerned according to a usual procedure.
  • the dispersion of the boehmite particles by the high-pressure emulsion is performed by putting the boehmite particles and water into a predetermined high-pressure emulsion apparatus and driving the apparatus concerned according to a usual procedure.
  • the high-pressure emulsion refers to the following operation.
  • the liquid containing the boehmite particles and the like is pressurized by a pump, passed through a narrow gap between a pulp sheet and a valve at a supersonic flow rate, and cavitation is thus generated at an edge portion of the pulp sheet. Then, a large pressure difference occurs locally following decay of cavities, and the aggregated particles in the liquid are torn off and redispersed into primary particles.
  • the organic solvent is not particularly limited as long as it is capable of dissolving the resin to be manufactured and of uniformly mixing the dissolved resin composition and the alumina particle composite therein in the polymerization process later.
  • THF tetrahydrofuran
  • dichloromethane 1,2-dichloroethane, chloroform, 1,1,2,2-tetrachloroethane, chlorobenzene, dichlorobenzene, methylethylketone, cyclohexanone, acetone and the like.
  • These organic solvents may be used singly or as a mixture of two or more thereof. It is tetrahydrofuran and chloroform that are particularly preferable.
  • a blended amount of water with 1 mol of the alumina particle composite is preferably 0.1 mmol or more in the organic solvent. In such a way, dispersibility of the alumina particles in the solvent can be improved.
  • a light transmittance of the dispersion liquid in which the alumina particles are dispersed be 40% or more.
  • the light transmittance is less than 40%, the dispersibility of the alumina particle composite is poor.
  • the alumina particle composite contained in the dispersion liquid cannot be dispersed uniformly in the target resin composition, thus sometimes making impossible to achieve the original object of the present invention.
  • the above-described alumina particle composite can be contained as the filler in a resin, and as a result, a predetermined resin composition can be obtained.
  • the blended amount of the alumina particle composite with the resin is not particularly limited as long as it allows required properties (rigidity, thermal resistance, thermal expansion resistance and the like) to be obtained.
  • the blended amount is preferably within a range from 1 to 50% by weight, more preferably 1 to 30% by weight.
  • the blended amount of the alumina particle composite is less than 1% by weight, an effect of blending the alumina particle composite is small, and in some case, the improvements of the properties such as the thermal resistance and the thermal expansion resistance are hardly recognized.
  • the blended amount of the alumina particle composite exceeds 50% by weight, not only the increase of the specific gravity cannot be ignored but also a disadvantage occurs in terms of cost, causing a problem that the cost and specific gravity of the resin composition is increased.
  • the content of the alumina particle composite is increased, the viscosity of the resin composition is increased, causing a deterioration of the moldability.
  • the resin made to contain the alumina particle composite can include polycarbonate resin, acrylic resin, methacrylic resin, polyester resin, styrene resin, amorphous olefin resin, and the like.
  • thermoplastic resin such as polycarbonate, acrylic and methacrylic resins are preferable.
  • the alumina particle composite is usable not for the purpose of improving the optical property but for the purpose of reinforcing the resin.
  • the alumina particle composite can be contained in the thermoplastic resin and thermosetting resin.
  • thermoplastic resin examples include polyolefin resin such as polyethylene resin, polypropylene resin and polybutylene resin, olefin modified resin such as maleic anhydride-modified polypropylene resin, polyester resin such as polyethylene terephthalate, polybutylene terephthalate and polytrimethylene terephthalate, styrene resin such as polystyrene, high impact polystyrene, AS resin (acrylonitrile-styrene resin), ABS resin (acrylonitrile-butadiene-styrene resin) and MBS resin (methylmethacrylate-butadiene-styrene resin), polyamide resin such as Nylon 6, Nylon 66 and Nylon 610, and further, polyoxymethylene, polyvinyl chloride, polycarbonate, polymethylene methacrylate, and thermoplastic polyimide.
  • polyolefin resin such as polyethylene resin, polypropylene resin and polybutylene resin
  • olefin modified resin such
  • thermosetting resin epoxy resin, phenol resin, xylene resin, alkyd resin, polyimide, urea resin, melamine resin, polyurethane resin, and the like can be mentioned.
  • resin to be selected is at least one thermoplastic resin selected from the polyolefin resin, the polyamide resin, the polyester resin, and the polystyrene resin.
  • the resin composition formed of polycarbonate can be obtained by a melt-mixing method of adding the alumina particle composite to the melted resin by using a twin screw mixer, a polymerization method of adding the alumina particle composite in a process of synthesizing a polymer from resin monomers, a solution method of mixing a liquid having the alumina particle composite uniformly dispersed therein with a solution having the resin dissolved therein and distilling away a solvent, and the like.
  • a solid of the alumina particle composite, a dispersion liquid thereof in water, or a dispersion liquid thereof in the organic solvent is used.
  • the mixer a twin screw extruder, a vacuum micro mixer/extruder, a labo-plasto mill, and the like are usable, and the mixer is selected and decided depending on the type of alumina particles and the type of solvent in which the alumina particles are dispersed.
  • the polycarbonate resin composition can be obtained by adding the alumina particles simultaneously with manufacturing of the polycarbonate resin by a so-called phosgene method, a so-called ester exchange method, or the like.
  • the phosgene method is a condensation reaction of a phenol compound with two or more valences with phosgene
  • the ester exchange method is an ester exchange reaction of carbonate diester and a hydroxyl compound.
  • the phenol compound with two or more valences is preferably 2,2-bis(4-hydroxydiphenyl)propane (common name: bisphenol A), bis(4-hydroxyphenyl)methane, bis(4-hydroxyphenyl)phenylmethane, bis(3,5-dimethyl-4-hydroxyphenyl)ethane, 1-phenyl-1,1-bis(4-hydroxyphenyl)ethane, 2,2-bis(3,5-dimethyl-4-hydroxyphenyl)propane, 1,1-bis(4-hydroxyphenyl)-3,3,5-trymethylchclohexane, bis(4-hydroxyphenyl)sulfone, 4,4′-dihydroxybenzophenone, more preferably, 2,2-bis(4-hydroxyphenyl)propane, 1,1-bis(4-hydroxyphenyl)-3,3,5-trimethylcyclohexane.
  • divalent phenols and the like may be used singly or in combination of two or more thereof.
  • the carbonate diester compound includes a diaryl carbonate such as diphenylcarbonate, and a dialkyl carbonate such as dimethylcarbonate and diethylcarbonate.
  • the hydroxy compound includes phenol, p-cresol, p-t-butylphenol, p-t-octylphenol, p-cumylphenol, bromophenol, tribromophenol, nonylphenol, and the like.
  • the phosgene is preferably used in the method for use in the phosgene method; however, it is possible to use other dihalogenated carbonyl, which does not inhibit the effect obtained by the present invention at all.
  • the polycarbonate is dissolved into the organic solvent having the alumina particle composite dispersed therein.
  • the polycarbonate is dissolved into the organic solvent, and the alumina particle composite dispersed in the organic solvent is mixed with the solution of the polycarbonate.
  • the mixed solution of the polycarbonate and the alumina particle composite is stirred well, followed by heating, thereby removing the solvent.
  • pressure reduction and heating are performed to the maximum possible, thereby distilling away the solvent quickly.
  • the viscosity of the solvent is raised; however, the stirring of the solution is to be continued until the stirring becomes impossible. In such a way, the resin composition free from aggregation can be obtained uniformly.
  • the organic solvent that can dissolve the polycarbonate well is recommended.
  • the organic solvent includes tetrahydrofuran, dichloromethane, 1,2-dichloroethane, chloroform, 1,1,2,2-tetrachloroethane, chlorobenzene, dichlorobenzene, methylethylketone, cyclohexanone, acetone, and the like.
  • the acrylic and methacrylic resin compositions in the thermoplastic resin can also be obtained by the melt-mixing method, the polymerization method, the solvent method and the like in a similar way to the polycarbonate resin composition.
  • (meth)acrylate esters such as methyl(meth)acrylate, ethyl(meth)acrylate, isopropyl(meth)acrylate, n-butyl(meth)acrylate, isobutyl(meth)acrylate, n-amyl(meth)acrylate, isoamyl(meth)acrylate, n-hexyl(meth)acrylate, 2-ethylhexyl(meth)acrylate, octyl(meth)acrylate, decyl(meth)acrylate, dodecyl(meth)acrylate), octadecyl(meth)acrylate, cyclohexyl(meth)acrylate, phenyl(meth)acrylate, benzyl(meth)acrylate.
  • (meth)acrylate esters such as methyl(meth)acrylate, ethyl(meth)acrylate, isopropyl(meth)acryl
  • methyl(meth)acrylate be a major component. More preferably, methyl(meth)acrylate is 70 mass % or more of the total amount of a monomer polymerizable with the aforementioned unsaturated monomer.
  • Samples and pure water were mixed and then treated with an ultrasonic cleaner for 15 minutes. Thereafter, the samples were applied to a hydrophilic carbon-coated collodion film on a copper mesh, followed by drying, thereby preparing observation samples. Electron microscope images of the samples were photographed with a transmission electron microscope (120 kV, 70 mA, 100 , 000 magnification) and observed.
  • TEM copper mesh Microgrid 150-B mesh, carbon-reinforced, Okenshoji Co., Ltd.
  • micrographs taken by the transmission electron microscope were scanned as electron data by a commercially available scanner, and the particle lengths were measured by using software to measure length on a commercially available personal computer.
  • the short and long axis lengths and thickness were respectively measured for 100 pieces selected at random.
  • Scion Image for Windows (registered trademark) manufactured by Scion corp.
  • Solid alumina particles obtained by freeze drying were put into epoxy resin, thus embedding the particles in the resin.
  • the cured resin was cut into thin sections with a thickness of about 60 to 100 nm by using an ultramicrotome at room temperature. Thereafter, the thin sections were attached to TEM grids, thereby preparing observation samples. Electron microscope images of the samples were photographed by a transmission electron microscope (300 kV, 400,000 magnification) and observed.
  • the samples were pressed on non-reflecting plates for measurement, thereby preparing observation samples.
  • the observation samples were measured by the X-ray diffractometer and compared with the JCPDS (Joint Committee on Powder Diffraction Standards) of alumina for identification.
  • the samples were observed by using TG-DTA, IR, and NMR.
  • TG-DTA measurement apparatus TG-DTA 320, manufactured by Seiko Instruments Inc.; Measurement temperature: room temperature to 900° C.; Temperature rise rate: 10° C./s
  • the obtained resin compositions were dried and granulated, followed by hot pressing, thereby obtaining sample films with a thickness of 2 mm.
  • the obtained sheets were measured in terms of the light transmittance, bending strength, flexural modulus, and linear expansion coefficient.
  • the light transmittance was measured by a haze meter (HM-65, manufactured by Murakami Color Research Laboratory).
  • the bending strength and flexural modulus were measured by an autograph (DSC-10T, manufactured by Shimadzu Corporation).
  • the linear expansion coefficient was measured by a thermomechanical analyzer (TMA120C, manufactured by Seiko Instruments Inc.).
  • the autoclaves were then moved to an oil bath and heated at 180° C. for 20 minutes (second heat treatment). Thereafter, the autoclaves were put into running water within 40 seconds, and were rapidly cooled to about 10° C. (third heat treatment). The third heat treatment was continued for 1 hour.
  • the autoclaves were put into the oven again and continued to be heated at 140° C. for 1 week (fourth heat treatment), and were then cooled with running water.
  • a supernatant of the solution in each autoclave was removed by centrifugation (18000 rpm, 30 min)
  • a sodium nitrate aqueous solution 0.5 M
  • centrifuge washed once with water
  • FIG. 3 is the exterior electron microscope photograph of the boehmite particles. The observed cross section along the short axis was hollow. This state is shown on a TEM photograph of a cross section in FIG. 4 .
  • the above-described operations were repeated a few times, thereby obtaining 3.32 g of the boehmite particles. Thereafter, the particles were put into about 100 g of water and stirred, and ultrasonic dispersion was carried out for 20 minutes by the ultrasonic dispersion apparatus. Thereafter, an obtained aqueous solution containing the boehmite particles was put into a high-pressure emulsifier, and was treated with a pressure of 50 MPa. The light transmittance measured at this time was 20%.
  • the ultrasonic dispersion was performed for 30 minutes by the ultrasonic dispersion apparatus, and a pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the light transmittance of the dispersion liquid of the boehmite particles in THF was increased to 72%.
  • Comparison of TEM images of the particles between a dispersed state into water and a dispersed state into THF revealed that the dispersion into THF relieved the aggregation more ( FIG. 5 ).
  • the dispersion liquid was concentrated and dried, and an amount of the paratoluenesulfonic acid on the particles was confirmed by using the TG-DTA. Then, 12 mmol of the paratoluenesulfonic acid was adhered with respect to 1 mol of the boehmite particles.
  • signals of the paratoluenesulfonic acid were able to be confirmed also by an IR measurement, a GC-MASS measurement and an NMR measurement.
  • Boehmite particles were obtained in a similar way to Example 1 except that the concentration of the sodium hydroxide was changed from 5.10 M to 4.80 M.
  • the pH of the solution obtained in the manufacturing process was 4.54.
  • the obtained boehmite particles were needle-like crystal with a long axis length of 350 ⁇ 37 nm, a short axis length of 5.5 ⁇ 0.5 nm, and an aspect ratio of about 45 to 80.
  • the observed cross section along the short axis had a hollow structure.
  • the dispersion liquid was concentrated and dried, and an amount of the paratoluenesulfonic acid on the particles was confirmed by using the TG-DTA. Then, 12 mmol of the paratoluenesulfonic acid was adhered with respect to 1 mol of the boehmite particles. Note that the signals of the paratoluenesulfonic acid were able to be confirmed also by the IR measurement, the GC-MASS measurement and the NMR measurement.
  • a colorless solid of the boehmite particles obtained by the method of Example 1 was put into an alumina crucible and heated at 1000° C. for 4 hours, thereby obtaining white powder. At this time, to prevent the hollow structure characteristic to the aforementioned boehmite particles from being broken by thermal stress, the temperature increase and decrease rate was set to 2° C./min.
  • the powder ( ⁇ alumina particles) was put into about 100 g of water and stirred well, and then the ultrasonic dispersion was carried out for 20 minutes by the ultrasonic dispersion apparatus. Thereafter, the aqueous solution containing the ⁇ alumina particles was put into the high-pressure emulsifier, and treated with the pressure of 50 MPa. The light transmittance measured at this time was 18%.
  • the ultrasonic dispersion was performed for 30 minutes by the ultrasonic dispersion apparatus, and a pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the light transmittance of the dispersion liquid of the ⁇ alumina particles in THF was increased to 65%.
  • the dispersion liquid was concentrated and dried, and an amount of the paratoluenesulfonic acid on the particles was confirmed by using the TG-DTA. Then, 6 mmol of the paratoluenesulfonic acid was adhered with respect to 1 mol of the ⁇ alumina particles. Note that the signals of the paratoluenesulfonic acid were able to be confirmed also by the IR measurement, the GC-MASS measurement and the NMR measurement.
  • a colorless solid of the boehmite particles obtained by the method of Example 2 was put into the alumina crucible and heated at 1000° C. for 4 hours (sintering treatment), thereby obtaining white powder.
  • the temperature increase and decrease rate was set to 2° C./min.
  • the ultrasonic dispersion was performed for 30 minutes by the ultrasonic dispersion apparatus, and a pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the light transmittance of the dispersion liquid of the ⁇ alumina particles in THF was increased to 58%.
  • the dispersion liquid was concentrated and dried, and an amount of the paratoluenesulfonic acid on the particles was confirmed by using the TG-DTA. Then, 6 mmol of the paratoluenesulfonic acid was adhered with respect to 1 mol of the ⁇ alumina particles. Note that the signals of the paratoluenesulfonic acid were able to be confirmed also by the IR measurement.
  • the ultrasonic dispersion was performed for 30 minutes by the ultrasonic dispersion apparatus, and the pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the light transmittance of the liquid became 45%.
  • a proper amount of ethyl acetate was put into 100 g (solid concentration of boehmite: 4.5% by weight) of the dispersion liquid of the boehmite particles containing the paratoluenesulfonic acid in THF, which was obtained by the method of Example 1. Subsequently, a mixture thus obtained was put into the centrifugal separator, and the centrifugation was performed therefor at 18000 rpm for 30 minutes. A supernatant was removed, and about 100 g of THF and 2.3 g of phenylboric acid were added to the liquid.
  • the ultrasonic dispersion was performed for 30 minutes by the ultrasonic dispersion apparatus, and the pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the pressure treatment of 50 MPa was performed by the high-pressure emulsifier.
  • the light transmittance of the liquid became 40%.
  • the temperature of the reaction system was increased to 260° C. over 30 minutes.
  • the mixture was stirred for about 30 minutes at a reduced pressure of 10 mmHg or less, thus reducing an oligomer component unreacted.
  • the mixture was ripened for 20 minutes in a range of 260° C. to 290° C. with the reduced pressure maintained, thereby obtaining a polycarbonate resin composition.
  • the obtained resin composition was dried and granulated, followed by hot pressing at 160° C., thereby obtaining a 2 mm thick plate.
  • the properties of the obtained sample plate was examined, and the light transmittance was 82%; the bending strength, 120 MPa; the flexural modulus, 4.5 GPa; the linear expansion coefficient, 5.8 ⁇ 10 ⁇ 5 /° C.; and the amount of particles blended, 8.7% by weight. These property values are shown in FIG. 8 , and an exterior appearance of the obtained transparent resin piece is shown in FIG. 7 .
  • the boehmite particle-dispersion liquid obtained in Example 2 the a alumina particle-dispersion liquids obtained in Examples 3 and 4, and the boehmite particle-dispersion liquids obtained in Examples 5 to 7 were used in place of the boehmite particle-dispersion liquid obtained in Example 1, thereby obtaining polycarbonate resin compositions in a similar procedure to that of Example 8.
  • These polycarbonate resin compositions were dried and granulated, followed by the hot pressing at 160° C., thereby obtaining plates with a thickness of 2 mm.
  • the obtained plates were measured in terms of the light transmittance and the bending strength in a similar way to Example 1. Results are shown in FIG. 8 .
  • Alumina sol 520 is commercially available as a dispersion liquid into water with a concentration of 20% by weight, Alumina sol 520 was used here as a dried solid by performing freeze drying therefor. Moreover, the particles have a boehmite structure and are stick-like or particle-like mixture with a particle diameter of 10 to 20 nm.
  • the temperature of the reaction system was increased to 230° C. over 30 minutes. At this temperature, the condensation was advanced for about 150 minutes at a reduced pressure of 5 mmHg or less while the mixture was being stirred. Furthermore, the temperature of the reaction system was increased to 260° C. over 30 minutes. At this temperature, the mixture was stirred for about 30 minutes at a reduced pressure of 10 mmHg or less, thus reducing the oligomer component unreacted. Finally, the mixture was ripened for 20 minutes in a range of 260° C. to 290° C. with the reduced pressure maintained, thereby obtaining a polycarbonate resin composition.
  • the obtained resin composition was dried and granulated, followed by the hot pressing, thereby obtaining a plate with a thickness of 2 mm.
  • the properties of the obtained sample plate were examined, and the light transmittance was 0%; the bending strength, 104 MPa; the flexural modulus, 3.3 GPa; the linear expansion coefficient, 6.3 ⁇ 10 ⁇ 5 /° C.; and the amount of particles blended, 9.4% by weight. Results are shown in FIG. 9 .
  • Polycarbonate resins were manufactured in a similar way to Comparative Example 1 except that Aluminum oxide C made by Nippon Aerosil Co., Ltd., alumina particles CAM 9010 made by Saint-Gobain Ceramic Materials K.K., and silica particles SNOWTEX MEK-ST made by Nissan Chemical Industries, Ltd. were used in place of Alumina sol 520 made by Nissan Chemical Industries, Ltd. Sample plates were made from these polycarbonate resins in a similar way to Comparative Example 1, and light transmittances thereof and the like were examined. Results are shown in FIG. 9 .
  • Aluminum oxide C made by Nippon Aerosil Co., Ltd. has a spherical shape with a diameter of about 13 nm.
  • alumina particles CAM9010 made by Saint-Gobain Ceramic Material K.K. have a rugby ball-like shape with a long axis length of about 90 nm and a short axis length of 10 to 15 nm. The particles do not exist singly, but four or five particles are linked together.
  • SNOWTEX MEK-ST made by Nissan Chemical Industries, Ltd. had a concentration of alumina at 30% by weight and was commercially available with alumina dispersed in methylethylketone. SNOWTEX MEK-ST was dried by spray drying and used as a solid. The particle diameter was about 10 to 20 nm.
  • Example 1 78 g of methyl methacrylate, 25 g of acrylic acid, and a proper amount of THF as a solvent were put into a flask in an inert gas stream, and 0.5 mol % of azobisisobutyronitrile (AIBN) as a polymerization initiator was added thereto. While the mixture was being heated to 80° C. and stirred, 258 g of the boehmite particle-dispersion liquid (concentration: 4.39% by weight) obtained in Example 1 was added thereto, and an obtained mixture was maintained at 80° C. as it was for 24 hours while being stirred.
  • AIBN azobisisobutyronitrile
  • the obtained product was returned to the room temperature and then added with excessive n-hexane, thereby precipitating a polymer, and then the polymer was filtered.
  • a methacrylate resin composition was obtained.
  • the obtained resin composition was dried and granulated, followed by the hot pressing, thereby obtaining a 2 mm thick plate.
  • the properties of the obtained plate were examined, and the light transmittance was 84%; the bending strength, 118 MPa; the flexural modulus, 4.3 GPa; the linear expansion coefficient, 5.5 ⁇ 10 ⁇ 5 /° C.; and the amount of particles blended, 9.2% by weight. These property values are shown in FIG. 8 .
  • Example 2 The boehmite particle-dispersion liquid obtained in Example 2 and the ⁇ alumina particle-dispersion liquids obtained in Examples 3 and 4 were used in place of the boehmite particle-dispersion liquid obtained in Example 1, thereby obtaining methacrylate resin compositions in a similar procedure to that of Example 15. These methacrylate resin compositions were dried and granulated, followed by the hot pressing, thereby obtaining plates with a thickness of 2 mm. The obtained plates were measured in terms of the light transmittance, the bending strength and the like in a similar way to Example 15. Results are shown in FIG. 8 .
  • the obtained resin composition was dried and granulated, followed by the hot pressing, thereby obtaining a 2 mm thick plate.
  • the properties of the obtained plate were examined, and the light transmittance was 0%; the bending strength, 106 MPa; the flexural modulus, 3.8 GPa; the linear expansion coefficient, 5.8 ⁇ 10 ⁇ 5 /° C.; and the amount of particles blended, 9.8% by weight. These property values are shown in FIG. 9 .
  • Methacrylate resin compositions were manufactured in a similar way to Comparative Example 5 except that Aluminum oxide C made by Nippon Aerosil Co., Ltd., alumina particles CAM 9010 made by Saint-Gobain Ceramic Material K.K., and silica particles SNOWTEX MEK-ST made by Nissan Chemical Industries, Ltd. were used in place of Alumina sol 520 made by Nissan Chemical Industries, Ltd. Sample plates were made from these resin compositions in a similar way to Comparative Example 5, and light transmittances thereof and the like were examined. Results are shown in FIG. 9 .
  • the resin composition containing the alumina particle composite of the present invention was excellent in light transmittance, bending strength, and flexural modulus, which revealed that both the transparency and the mechanical strength were excellent.
  • the linear expansion coefficient of the resin composition was also low, which revealed that thermal stability thereof was also excellent.
  • Example 6 paratoluenesulfonic acid bonded to the surfaces of the alumina particles was substituted by phenylboric acid, thereby preparing the alumina particle composite in which phenylboric acid was chemically bonded to the surface.
  • alumina particle composite containing phenylboric acid also by the method as described in Example 5
  • a liquid in which the dispersibility of alumina is higher can be obtained than in the case using the method of Example 5.
  • the resin composition of the present invention is, when necessary, can be added with an antioxidant, a thermal stabilizer, an ultraviolet absorber, a lubricant, a mold release agent, dyestuff, a colorant including pigment, an attachment agent of an additive, a nucleating agent, and the like singly or in proper combination.
  • the oxidant and thermal stabilizer are hindered phenol, hydroquinone, thioether, phosphates, substitutions thereof, or the like.
  • the ultraviolet absorber is resorcinol, salycylate, benzotriazole, benzophenone, and the like.
  • the lubricant and mold release agent are silicone resin, montanic acid or salts thereof, stearic acid or salts thereof, stearyl alcohol, stearyl amide, or the like.
  • the dyestuff is nitrosin or the like.
  • the pigment is cadmium sulfide, phthalocyanine, or the like.
  • the attachment agent is silicone oil or the like.
  • the nucleating agent is talc, caolin, or the like.

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US20100210777A1 (en) * 2004-09-07 2010-08-19 Nissan Motor Co., Ltd. Alumina particle composite, method of manufacturing the alumina particle composite, resin composition and method of manufacturing the resin composition
US20100239835A1 (en) * 2007-10-02 2010-09-23 Gian Paolo Ferraro Polymeric film and optical device comprising said film
US20100256270A1 (en) * 2007-07-17 2010-10-07 Nissan Motor Co., Ltd. Polycarbonate resin composition and process for producing the same
USRE43468E1 (en) 2004-08-26 2012-06-12 Nissan Motor Co., Ltd. Alumina particles of high aspect ratio, alumina particle manufacturing method, resin composition, and resin composition manufacturing method
US8278382B2 (en) 2008-12-08 2012-10-02 Renault S.A.S. Method for preparing a transparent polymer material including mineral nanoparticles with a shape factor strictly higher than 1.0
US20130306912A1 (en) * 2012-05-18 2013-11-21 Research & Business Foundation Sungkyunkwan University Yttrium aluminum garnet phosphor and synthesis method thereof
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JP5140930B2 (ja) * 2006-02-17 2013-02-13 日産自動車株式会社 金属酸化物粒子複合体、それを用いた樹脂複合材、及びそれらの製造方法
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