WO2007105466A1 - 粉砕媒体を用いる粉末粒子の製造方法 - Google Patents
粉砕媒体を用いる粉末粒子の製造方法 Download PDFInfo
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- WO2007105466A1 WO2007105466A1 PCT/JP2007/053465 JP2007053465W WO2007105466A1 WO 2007105466 A1 WO2007105466 A1 WO 2007105466A1 JP 2007053465 W JP2007053465 W JP 2007053465W WO 2007105466 A1 WO2007105466 A1 WO 2007105466A1
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Classifications
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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
- 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
- C09C1/0015—Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C17/00—Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
- B02C17/18—Details
- B02C17/20—Disintegrating members
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B02—CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
- B02C—CRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
- B02C18/00—Disintegrating by knives or other cutting or tearing members which chop material into fragments
- B02C18/06—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives
- B02C18/14—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives within horizontal containers
- B02C18/148—Disintegrating by knives or other cutting or tearing members which chop material into fragments with rotating knives within horizontal containers specially adapted for disintegrating plastics, e.g. cinematographic films
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C12/00—Powdered glass; Bead compositions
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
Definitions
- the present invention relates to a method for producing powder particles using a grinding medium.
- Fine particle production methods are roughly classified into two types: a bottom-up method in which fine particles are generated by nuclear growth and the like, and a top-down method in which fine particles are generated by pulverizing a large lump. From the viewpoint of excellent mass productivity, the top-down method is often used.
- One of the methods for obtaining fine particles by the top-down method is a medium grinding method in which grinding is performed using a medium. For example, in a ball mill using ceramic balls or the like as a medium, powder balls such as zirconium or the like, ground materials, solvents, and dispersing agents as necessary are added to the container, and the pulverized balls are rotated by rotating the container.
- Patent Document 1 JP-A-9 253517 (Claim 1 etc.)
- An object of the present invention is to provide a method for producing particles having an average particle size on the order of submicrons despite having an amorphous structure.
- the present invention is a method for producing powder particles that obtains powder particles by pulverizing an object to be pulverized using a plurality of types of pulverization media, and is 0% relative to the average particle diameter of the object to be crushed before pulverization .
- a method for producing powder particles using a grinding medium comprising at least one kind (grinding medium A) having an average particle diameter of 01 to 5 times and at least one kind (grinding medium B) having an average particle diameter of 10 to 450 times It is.
- the average particle size of the material to be pulverized and the pulverization medium A means the arithmetic average particle size.
- the average particle size of grinding media B means a cumulative 50% particle size (D), which is
- FIG. 1 is an SEM photograph of alkali glass crushed by a conventional method.
- FIG. 2 SEM photograph of alkali lath pulverized by the method of the present invention.
- an average particle size of 0.01 to 5 times the average particle size before pulverization of the material to be crushed A fine grinding medium (grinding medium A) having an average particle diameter of 10 to 450 times is used as another type, and a grinding medium (grinding medium B) to which a load is applied is used.
- a material to be crushed is pulverized using a medium, a ball mill, a bead mill, a planetary ball mill, or the like is used, and as the pulverizing medium A and pulverizing medium B, pulverized balls, pulverized beads, or the like are used.
- the grinding medium A includes silica, zirconium, yttria, ceria, magnesia, zinc oxide, manganese oxide, copper oxide, and oxidation. Oxides such as iron, holmium oxide, lead oxide and tin oxide, and those having a load softening point higher than the firing temperature and a high load soft spot glass force can also be used.
- the material used later together with the material to be pulverized and the material constituting the composition together with the material to be pulverized are preferable.
- the material to be crushed is a low-load soft spot glass used for a field emission display paste, which will be described later
- an acid that can be used as a filler component in the paste for the grinding media examples include pottery and high-load soft spot glass. This is an aspect that acts as a medium when pulverizing the material to be crushed, can be mixed into the composition without removing the medium, and later acts as a filler component.
- a pulverizing medium such as an acid or high-load soft point glass, which acts to pulverize the low load soft point glass, which is the object to be pulverized, to a size of submicron order.
- a filler component when producing a composition that is not removed, the process can be simplified.
- the present invention by using the grinding medium A satisfying the average particle size ratio in the above range, that is, for the material to be ground before grinding, compared with the grinding media conventionally used.
- the working point of grinding can be dramatically increased.
- the grinding medium B satisfying the average particle size ratio in the above range applies a large load to the grinding medium A, a large shearing force can be generated.
- a grinding medium having a large particle size was used.
- the increase in the working point of the grinding and the increase in the shear force at the working point are contrary to each other in the conventional grinding method.
- the resulting powerful effect can be obtained simultaneously, and as a result, particles having an average particle size on the order of submicrons can be obtained.
- the above average particle diameter ratio of the grinding medium A is smaller than 0.01 times, as a result, it is too light for the material to be ground, so that the shearing force necessary for grinding cannot be obtained. More preferably, it is 0.1 times or more. On the other hand, if the average particle size ratio is larger than 5 times, particles having an average particle size on the order of submicrons with few action points cannot be obtained. More preferably, it is 1 time or less.
- the average particle size ratio of the grinding medium B is less than 10 times, as a result, it becomes too light and sufficient shearing force cannot be obtained. For more efficient pulverization, 100 times or more is preferable. On the other hand, if the average particle size ratio is larger than 450 times, a sufficient working point with the grinding medium A cannot be obtained, and particles having an average particle size of submicron order cannot be obtained. For more efficient grinding, 300 times or less is preferable.
- Examples of methods for measuring the average particle size of the object to be crushed and the grinding media A and B include a method of measuring with a light scattering device and the like, a method of calculating the image analysis power of a micrograph, and the like.
- a method of measuring with a light scattering device and the like there is no problem if the fine particles are not secondary agglomerated, but in the case of secondary agglomeration, it is difficult to measure the average particle size of the primary particles. There's a problem. Therefore, in the case of the present invention, it is preferable to use a value that also calculates the image analysis power of the micrograph for the average particle size of the object to be crushed and the grinding medium A.
- this method can obtain a value reflecting the average particle size of the primary particles.
- the photographic power obtained by observation with a scanning electron microscope (Hitachi, Ltd. S 4800, etc.) is also measured for particles that can be measured within the field of view and averaged.
- the method for measuring the average particle diameter of the grinding medium B is preferably a method using a light scattering device or the like because there is almost no secondary aggregation.
- the average particle size can be measured using a particle size distribution measuring device (Microtrack 9320HRA manufactured by Nikkiso Co., Ltd.).
- the material to be ground and the grinding medium can be distinguished by the Vickers hardness, and the material having the smallest Vickers hardness is defined as the material to be ground.
- the Vickers hardness can be measured according to the test force 9.807N, according to the “Fine ceramics hardness test method (JIS R1610: 2003)”, and the average of the five measured values is the Vickers hardness. Can be used.
- the weight of the grinding medium B1 is preferably heavier than the weight of the grinding medium A1.
- the grinding medium A is added in the range of 1: 0.1 to LOO, where the total volume of the material to be ground is 1.
- the volume ratio of the grinding medium A is less than 0.1, there may be a case where a sufficient working point cannot be obtained even if the average particle size is small, and if it is more than 100, the amount of the material to be ground is too small.
- the yield of the obtained particles may be small.
- the range of 1: 0.1 to 30 is preferable in that the average particle size can be reduced in a short time with good yield.
- the grinding medium B is preferably added in the range of 1: 0.1 to LOO, where the total volume of the material to be ground and the grinding medium A is 1. If the volume ratio of grinding media B is less than 0.1 in the mixture, the purpose of applying a load to grinding media A cannot be achieved. Not right. More preferably, it is 1: 2.5-20. In the case of the wet method, it is preferable to add at least until the material to be ground, grinding medium A, and grinding medium B are immersed in the solvent.
- examples of the material to be crushed include glass, ceramics, carbon-based materials, pigments, and the like.
- the present invention is preferably used particularly when the material to be crushed is inorganic particles such as glass and ceramics.
- the inorganic particles preferably have an average particle size before pulverization of 0.1 to LOOO / zm. 0.: When smaller than L m, the average particle size is sufficiently small, so there is no need for further pulverization. Such small powder particles are produced by the bottom-up method. On the other hand, when the average particle size before pulverization is larger than 1000 m, it is not preferable because pulverized balls such as zirconia that can be used as the pulverizing medium B are difficult to obtain. The present invention is particularly effective when the average particle size of the inorganic particles before pulverization is more than 0.7 / zm and not more than 10 m.
- the load softening point is 300 ⁇ Glass with a specific temperature of 500 ° C or glass with a specific gravity of 2 to 4 can be crushed by conventional methods, and can be flattened to obtain particles having the desired average particle size on the order of submicrons. It was difficult. This is because the glass having the above-mentioned properties is sticky during pulverization, and the crushed shape becomes flat due to the stickiness and absorbs shearing force.
- a low-load softening point glass object to be crushed
- pulverization medium A solvent
- a dispersant as required are weighed and mixed to obtain a mixture so as to obtain a predetermined mixing ratio, and ultrasonic waves are obtained.
- an oxide or a high-load soft spot glass that can be used as a filler when preparing the composition later is prepared.
- oxides include silica, alumina, titer, zirconium, yttria, ceria, magnesia, zinc oxide, manganese oxide, copper oxide, iron oxide, zinc oxide, lead oxide, and tin oxide. It is done.
- the powder frame medium A may be used in combination of two or more types, and the combination thereof is not particularly limited.
- any of water, alcohol, and an organic solvent can be used, and these may be used in combination.
- the solvent any of water, alcohol, and an organic solvent can be used, and these may be used in combination.
- the pulverized material when the pulverized material that has been powdered by drying the solvent after pulverization is collected, the pulverized material often undergoes secondary aggregation during drying. Therefore, using the solvent used in the composition to be prepared, store it in a slurry state, It is convenient to use as it is without drying in order to suppress secondary aggregation of the material to be crushed. Therefore, it is preferable to select a solvent that does not need to go through a drying step after pulverization.
- an anionic surfactant As the dispersant, an anionic surfactant, a cationic surfactant, a nonionic surfactant, an amphiphilic polymer, a comb polymer, or the like can be used.
- a dispersing agent As the particles become smaller due to grinding, secondary agglomeration is likely to occur because the new surface that appears by grinding is active. As secondary agglomeration progresses, the energy of pulverization is used to disintegrate secondary agglomeration, which may lead to a phenomenon in which further particle size reduction becomes impossible. However, if a dispersing agent is added, the dispersing agent is quickly adsorbed on the activated surface, and secondary aggregation can be suppressed.
- the total concentration of the mixture of the material to be ground and grinding medium A is preferably 5 to 40 vol%. If the amount is less than 5 vol%, the yield of fine particles obtained tends to be small because the amount of the object to be crushed is too small. It is difficult to obtain the shearing force necessary for crushing. More preferably, it is 1 O-30 vol%.
- the mixture of the material to be pulverized, the pulverizing medium A, the dispersant, and the solvent is put into a pulverizing container made of zirconia or the like.
- a pulverizing ball made of zirconium or the like is added as pulverizing medium B in the range of 1: 0.1 to LOO, where the total volume of the pulverized material and pulverizing medium A is 1.
- the grinding medium B is not immersed in the solvent, the solvent is added until the grinding medium B is immersed.
- the grinding medium B is preferably made of the same material as the grinding container.
- the following is a mixture of the above mixed liquid and the pulverizing medium B added.
- the centrifugal force exerted on the grinding medium by rotation and revolution is preferably 1G or more when the acceleration of gravity is G in the vertical direction of the side surface of the grinding container. More preferably 4G or more. If it is less than 1 G, the shearing force required for pulverization does not act on the point of action between the media, and it is difficult to obtain particles having an average particle size of the desired submicron order.
- the grinding medium B is removed from the grinding solution, and the grinding medium A is removed as necessary.
- Grinding media B can be removed through a filter. If the removal rate of the pulverized solution with a high viscosity filter is slow, pulverizing medium B is removed by pressure filtration or suction filtration. When removing grinding media A, density, solubility, etc. can be used. When the density of pulverizing media A and the material to be crushed are different, they can be separated by centrifugal separation or air classification after drying.
- the density is smaller than that of zirconia used as the pulverizing medium A, and therefore a separation method by centrifugal separation or air classification after drying can be used.
- the grinding medium A and the material to be ground are different in solubility, they can be separated by dissolving only the grinding medium.
- the material to be ground is not soluble in acid, if a metal is used for grinding medium A, grinding medium A can be removed by dissolving the metal with acid.
- the powder particles comprising the material to be pulverized manufactured by the method as described above can be used in a composition suitable for fine processing.
- a composition suitable for fine processing for example, (1) compositions used as circuit materials, (2) plasma display members such as dielectrics and partition walls, field emission display members such as insulating layers and electron emission layers, and surface conduction displays such as insulating layers Examples thereof include compositions used for display members such as members.
- components of the composition it is preferable to include powder particles made of a material to be crushed produced by the method of the present invention, a binder resin and a solvent.
- fillers may be included.
- the composition may contain a carbon-based material.
- the carbon-based material include carbon nanotubes, carbon nanohorns, carbon nano coinole, fullerene, and carbon black.
- the composition when used for a field emission display, it preferably contains carbon nanotubes, carbon nanohorns, and carbon nanocoils that can emit electrons by applying voltage in a vacuum.
- the one-bonn nanotube is most suitable for use because it has higher electron emission capability than carbon nanohorn and carbon nanocoil.
- a carbon nanotube paste for field emission will be described as an example of a composition containing powder particles produced by the method of the present invention.
- the powder particles obtained by the above method are glass.
- Carbon nanotube paste for field emission is used as an electron emission source. Includes Bonn Nanotube (hereinafter referred to as CNT), glass, binder resin, solvent, etc.
- CNT single-layer or multi-layer CNTs such as two layers and three layers can be used. Mix CNTs with different numbers of layers.
- Glass (the above powder particles) is necessary for imparting adhesion between the CNT and the force sword substrate.
- the average particle size of the glass used is preferably 50 nm to 700 nm. If it is smaller than 50 nm, a strong matrix is not formed, and if it is larger than 700 nm, the surface unevenness becomes large, which causes non-uniform electron emission. More preferably, it is 70 nm-600 nm.
- the load softening point of the glass used for the carbon nanotube paste for field emission is preferably 500 ° C or less. This is because soda lime glass can be used as a glass substrate on which an electron emission source, a partition wall and the like are provided when a glass having a load softening point of 500 ° C or lower is used. When the load soft spot exceeds 500 ° C, the glass substrate shrinks, and pattern displacement, warpage, and cracking are likely to occur. Therefore, the glass are use the carbon nanotube paste for field E mission is preferably from 45 to 86 weight 0/0 containing Bi O. This will load the glass
- the glass tends to crystallize, which is not preferable. More preferably, it is 70 to 85% by weight.
- thermomechanical analyzer for example, EX TER6000 TMAZSS, manufactured by Seiko Instruments Inc.
- the glass load soft spot is 10g each on the glass rod and the quartz glass rod of the standard sample.
- the glass powder if it is 45 to 86 weight 0/0 containing Bi O, the other compositions, especially
- Bi O of from 45 to 86 weight 0/0, 0.5 to 8 wt 0/0 of SiO,. 3 to
- the load softening point of the glass becomes too high. More preferably, it is 0.5 to 2% by weight.
- the stability of the glass can be improved.
- the load softening point of the glass becomes too high. More preferably, it is 3 to 10% by weight.
- ZnO may not be included, but the load softening point can be reduced by adding up to 25% by weight. If it exceeds 25% by weight, the glass tends to crystallize, which is not preferable. More preferably 5 to 15 weight 0/0.
- the compositional components of the glass can be analyzed as follows. First, inorganic qualitative analysis is performed using a fluorescent X-ray analyzer (for example, energy dispersive fluorescent X-ray analyzer MESA-500, manufactured by Horiba, Ltd.). Subsequently, the detected element can be quantitatively analyzed with an ICP emission analyzer (for example, ICP emission analyzer SPS3000, manufactured by SII Nano Technology Co., Ltd.) to determine the composition. In addition, elements that cannot be detected in principle by X-ray fluorescence analysis (Li, B) and insensitive elements (Na, Mg, etc.) are also examined. If they are the main components, they are quantified together with an ICP emission spectrometer. .
- a fluorescent X-ray analyzer for example, energy dispersive fluorescent X-ray analyzer MESA-500, manufactured by Horiba, Ltd.
- ICP emission analyzer for example, ICP emission analyzer SPS3000, manufactured by SII Nano Technology Co., Ltd.
- the binder resin used in the carbon nanotube paste for field emission includes cellulosic resin (ethyl cellulose, methyl cellulose, nitrocellulose, cetinoresenolellose, senorelose propionate, hydroxypropinoresenorelose).
- cellulosic resin ethyl cellulose, methyl cellulose, nitrocellulose, cetinoresenolellose, senorelose propionate, hydroxypropinoresenorelose.
- the solvent used in the carbon nanotube paste is preferably a solvent that dissolves the organic components contained in the paste.
- a solvent that dissolves the organic components contained in the paste.
- polyhydric alcohols such as diols and triols typified by ethylene glycol and glycerin, compounds obtained by etherification and esterification of alcohols (ethylene glycol monoalkyl ether, ethylene glycol resinalequinoleateol, And ethylene glycol-norenorequinoleateolate acetate, ethylene glycol monoalkyl ether acetate, diethylene glycol dialkyl ether, propylene glycol monoalkyl ether, propylene glycol dialky ether, propylene glycol alkyl ether acetate).
- terbinol ethylene glycol monomethyl ether, ethylene glycol monoethyl eno enoate, ethylene glycol mono mono propino enoate, ethylene glycol mono butyl ether, diethylene glycol dimethyl ether, jet ethylene glycol eno tie
- Ethylene Glycono Resin Mouth Pinoleetenore Diethylene Glycolinole Resin Tinoreate
- Tenole Methyl Cesolve Solv Acetate, Ethyl Selcol Solvacetate, Propyl Cellosolve Acetate, Butyl Selcol Solve Acetate, Propylene Glycol Monoremonomethinorete Tenole Acetate, Propylene Glycol Noremono echinoreethenoleacetate, propylene glycol monopropyl ether acetate, 2, 2, 4 trimethyl -1,3-Pentanediol monoisobutyrate, butyl carbitol acetate
- the carbon nanotube paste for fine red emission may contain a dispersant or the like as appropriate in addition to CNT, glass, binder resin, and solvent.
- the dispersant used for the carbon nanotube paste is preferably an amine-based comb block copolymer.
- amine-based comb block copolymers include Solvase 13240, Solsose 13650, Solsparse 13940, and Solsparth manufactured by Abyssia Co., Ltd. 24000SC, Sonoreth Nose 24000GR, Sonoreth Noose 28000 (1 /, Misaki quotient name), and so on.
- the carbon nanotube paste for field emission may be imparted with photosensitivity, and by containing a photosensitive organic component, pattern processing can be performed through exposure and development.
- a photosensitive organic component a chemical change occurs when irradiated with ultraviolet rays, so that a negative type photosensitivity that becomes soluble in the developer before exposure to ultraviolet light but becomes insoluble in the image solution after exposure.
- the negative photosensitive organic component contains at least one photosensitive component selected from a photosensitive polymer, a photosensitive oligomer, and a photosensitive monomer, and further, if necessary, binder resin, light As a polymerization initiator, ultraviolet light absorber, sensitizer, sensitizer, polymerization inhibitor, plasticizer, thickener, antioxidant, dispersant, organic or inorganic precipitation inhibitor, leveling agent, etc. It is also preferable to add ingredients that act.
- the photosensitive polymer used in the carbon nanotube paste for field emission generally has a function of binder resin.
- the photosensitive polymer preferably has a carboxyl group.
- Polymers having a carboxyl group include, for example, monomers containing carboxyl groups such as acrylic acid, methacrylic acid, itaconic acid, crotonic acid, maleic acid, fumaric acid, bulacetic acid, or acid anhydrides thereof, methacrylic acid esters, acrylic acid, and the like. It can be obtained by selecting monomers such as acid ester, styrene, acrylonitrile, vinyl acetate, 2-hydroxy acrylate, and copolymerizing using an initiator such as azobisisobutyl-tolyl.
- a copolymer having (meth) acrylic acid ester and (meth) acrylic acid as a copolymerization component is preferably used because of its low thermal decomposition temperature upon firing.
- styrene Z methyl methacrylate Z methacrylic acid copolymer is preferably used.
- the succinic acid value of the copolymer having a carboxyl group is preferably 50 to 150 mgKOHZg.
- the acid value is larger than 150, the allowable development width becomes narrow. Also, the acid value is less than 50 Then, the solubility with respect to the developing solution of an unexposed part falls. When the developer concentration is increased, peeling occurs to the exposed area, and a high-definition pattern is obtained.
- the photosensitive polymer preferably has an ethylenically unsaturated group in the side chain.
- an ethylenically unsaturated compound or acrylic acid having a glycidyl group or an isocyanate group with respect to a mercapto group, amino group, hydroxyl group or carboxyl group in the polymer There is a method in which a carboxylic acid such as chloride, methacrylic acid chloride or aryl chloride, maleic acid is reacted.
- Examples of the ethylenically unsaturated compound having a glycidyl group include glycidyl acrylate, glycidyl methacrylate, allyl glycidyl ether, glycidyl ethyl acrylate, crotonyl glycidyl ether, crotonic acid glycidyl ether, and isocrotonic acid glycidyl ether.
- the structure CH C (CH) COOCH CHOHCH—
- the compound which has is used preferably.
- Examples of the ethylenically unsaturated compound having an isocyanate group include (meth) attalyloyl isocyanate and (meth) attaroyl ethyl isocyanate.
- ethylenically unsaturated compounds having a glycidyl group or an isocyanate group, acrylic acid chloride, methacrylic acid chloride or aryl chloride are 0.05 to 1 to the mercapto group, amino group, hydroxyl group and carboxyl group in the polymer. It is preferable to carry out a molar equivalent reaction.
- Preparation of an amine compound having an ethylenically unsaturated bond is carried out by using a glycidyl (meth) acrylate, (meth) acrylic acid chloride, (meth) acrylic anhydride, etc. having an ethylenically unsaturated bond as an amino compound. ⁇ ⁇ ! A plurality of ethylenically unsaturated group-containing compounds may be mixed and used.
- a compound containing a carbon-carbon unsaturated bond having photoreactivity can be used.
- alcohols for example, ethanol, propanol, hexanol, Acrylic esters or methacrylate esters of octanol, cyclohexanol, glycerin, trimethylolpropane, pentaerythritol, etc.
- carboxylic acids eg, acetic acid propionic acid, benzoic acid, acrylic acid, methacrylic acid
- Succinic acid maleic acid, phthalic acid, tartaric acid, succinic acid, etc.
- amide derivatives eg acrylamide, methacrylamide, N-
- One type or two or more types of photosensitive monomers can be used.
- the photosensitive monomer is preferably added in the range of 2 to 40% by weight, more preferably 5 to 30% by weight, based on the total photosensitive organic component. If the amount of the photosensitive monomer is too small, the photocuring will be insufficient, and the sensitivity of the exposed part will be lowered or the development resistance will be lowered. If the amount of the photosensitive monomer is too large, the solubility of the unexposed portion in water may be lowered, or the crosslinking density may be too high, which may cause debinding failure during firing.
- the photopolymerization initiator used for the carbon nanotube paste for field emission is selected from those generating radical species.
- Photoinitiators include: (a) Jetoxyacetophenone, 2-hydroxy-2-methyl 1-phenolpropane 1-one, benzyldimethyl ketal, 1- (4-isopropylphenyl) 2 hydroxy-2-methylpropanone 1— ON, 4— (2-hydroxyethoxy) phenol (2-hydroxy-1-propyl) ketone, 1-hydroxycyclohexyl roofing ketone, 1 phenol 1,2-propanedione 2— (o ethoxycarbo- L) oxime, 2-methyl- [4 (methylthio) phenol] — 2-morpholinopropane— 1-one, 2-benzyl-2-dimethylamino— 1— (4 morpholinophenol) monobutanone, 1, benzoin , Benzoin methyl ether, benzoin ethyl ether, benzoin isopropyl ether, benzo
- the photopolymerization initiator is added in the range of 0.05 to 10% by weight, more preferably 0.1 to 10% by weight, based on the photosensitive organic component. If the amount of the photopolymerization initiator is too small, the photosensitivity becomes poor. If the amount of the photopolymerization initiator is too large, the residual ratio of the exposed portion may be reduced.
- the sensitivity can be improved and the effective wavelength range for the reaction can be expanded.
- the sensitizer include 2,4 dimethylthioxanthone, 2,4 jetylthioxanthone, 2-isopropylthioxanthone, 2,3 bis (4 jetylaminobenzal) cyclopentanone, 2, 6 Bis (4 dimethylaminobenzal) cyclohexanone, 2, 6-Bis (4-dimethylaminobenzal) 4-Methylcyclohexanone, Michler's ketone, 4, 4 —Bis (jetylamino) benzophenone, 4, 4—Bis (Dimethylamino) chalcone, 4, 4—bis (jetylamino) chalcone, p dimethylaminocinnamylidene indanone, p dimethylaminobenzylidene indanone, 2— (p dimethylaminophenol bilene) isonaft thiazole, 1,3 bis (4-dimethylaminophenol) -naphthoazole, 1,3
- sensitizers can be used. Some sensitizers can also be used as photopolymerization initiators. When the sensitizer is added to the photosensitive paste, the addition amount is usually 0.05 to 10% by weight, more preferably 0.1 to 10% by weight, based on the photosensitive organic component. If the amount of sensitizer is too small, the effect of improving photosensitivity If it is not exhibited and the amount of the sensitizer is too large, the residual ratio of the exposed portion may be reduced.
- the carbon nanotube paste for field emission can be prepared by preparing various components so as to have a predetermined composition and then homogeneously mixing and dispersing them in a kneader such as a three-roller, ball mill, or bead mill. .
- the paste viscosity is adjusted as appropriate depending on the addition ratio of glass, thickener, organic solvent, plasticizer, suspending agent, etc., but when pattern coating is performed using the slit die coater method or screen printing method.
- the range is preferably 2 to 200 Pa's.
- pattern processing is performed by spin coating or spraying, 0.001 to 5 Pa's is preferable.
- a back substrate is fabricated.
- a conductive sword electrode is formed by depositing a conductive film such as ITO on a glass substrate such as PD200 manufactured by Asahi Glass Co., Ltd., which is heat-resistant glass for soda glass or PDP.
- an insulating material is produced by laminating 5 to 15 m of an insulating material by a printing method.
- a gate electrode layer is formed on the insulating layer by vacuum deposition.
- An emitter hole pattern is formed by resist coating on the gate electrode layer and etching the gate electrode and the insulating layer by exposure and development.
- the composition containing the powder particles obtained by the present invention (the carbon nanotube paste for field emission) is applied by screen printing or a slit die coater. Development is performed after top exposure or back exposure, and an electron emission source pattern is formed in the emitter hole and baked at 400 to 500 ° C.
- the CNT film is brushed by laser irradiation or tape peeling.
- An anode electrode is formed by depositing ITO on a glass substrate such as soda lime glass or PD200 manufactured by Asahi Glass Co., Ltd., which is heat resistant glass for PDP. Red, green and blue phosphors are laminated on the anode electrode by printing.
- the triode-type electron-emitting device can be manufactured by pasting the back substrate and the front substrate together with a spacer glass and evacuating them with an exhaust pipe connected to the container.
- voltage of 1 to 5 kV is applied to the anode electrode
- electrons are emitted from the CNTs and phosphor emission can be obtained.
- the electron-emitting device manufactured in this manner can be used as a liquid crystal backlight by attaching a drive driver and installing it on the back surface of the liquid crystal panel.
- a drive driver when attached to an electron-emitting device in which red, green, and blue phosphors are printed for each pixel, it can be used as a field emission display.
- the material to be ground and the grinding medium A were mixed in the materials and proportions described in Tables 1 to 5, and a mixture was prepared using terbineol as a solvent so that the material to be ground was 20% by weight. Subsequently, 90 ml of the mixed solution was charged into a Dino mill (manufactured by Shinmaru Enterprises Co., Ltd.) filled with grinding medium B described in Table 1 and filled with 85% by volume (510 ml) of the vessel volume. After clogging the liquid feeding port and waste liquid port of the vessel and sealing the pulverized solution in the vessel, grinding was performed for 180 minutes with a 64 mm ⁇ agitator disk at a peripheral speed of 10.5 m / s. After pulverization, suction filtration was performed using a mesh filter of S US # 150 to remove pulverization medium B from the pulverized solution.
- Example 26 In Example 26 and Comparative Example 8, the surface roughness was measured by the following method.
- the surface roughness Ra of the surface of the electron-emitting device was measured with a stylus according to JIS B0601-1982 using Surfcom 1400 manufactured by Tokyo Seimitsu Co., Ltd.
- R ⁇ A-rX 2 / V (X 2/3 + X 2/3 ) ⁇ / ⁇ X
- A is the average particle size of the mixture of the material to be ground and grinding media A
- r is the average particle size of grinding media A
- the average particle size of the grinding medium B was measured using a particle size distribution measuring device (manufactured by Nikkiso Co., Ltd., Microtrac 9 320HRA).
- the average particle size measured by the particle size distribution measuring device is the cumulative 50% particle size (D).
- Glass 1 Bismuth glass (bismuth oxide: 50 wt%, boron oxide: 21 wt%, silicon oxide: 7 wt%, zinc oxide: 22 wt%), load softening point 447 ° C, average particle size 0.8 m, pickers Hardness 5GPa
- Glass 2 Alkaline glass (boron oxide: 35 wt%, aluminum oxide: 22.7 wt%, oxide silicon: 12.9 wt%, lithium oxide: 12.4 wt%, magnesium oxide: 6.4 wt%, oxide Barium: 4.2 wt%, calcium oxide: 4. lwt%, zinc oxide: 2.3 wt%), soft load point 458.
- C average particle size 1. l ⁇ m, Vickers hardness 5GPa
- Glass 3 Bismuth glass (bismuth oxide 75 wt%, boron oxide 7 wt%, silicon oxide 2 wt%, zirconium oxide 12 wt%) Glass load softening point 380 ° C, average particle size 2 .: L m, bit Curse hardness 4GPa
- Glass 4 Bismuth glass (bismuth oxide: 75 wt%, boron oxide: 0.9 wt%, silicon oxide: 1.9 wt%, zinc oxide: 12 wt%, aluminum oxide: 0.2 wt%, sodium oxide: 4 w t %), Load softening point 394 ° C, average particle size 5 ⁇ m, Vickers hardness 4GPa
- Glass 5 Bismuth-based glass (bismuth oxide: 85 wt%, boron oxide: 4 wt%, silicon oxide: 1.5 wt%, zinc oxide: 9.5 wt%), load softening point 415 ° C, average particle size 9 ⁇ m , Pitzkers hardness 4.5 GPa
- Powdered medium A1 Titer (average particle size 0.013 m, Vickers hardness 7.5 GPa, Nippon Aerosil Co., Ltd. aluminum oxide C)
- Powdered medium A2 Alumina (average particle size 0.021 111, Vickers hardness 150? &, Titanium dioxide P25 manufactured by Nippon Aerosil Co., Ltd.)
- Grinding media A3 Titer (average particle size 0.051 m, Pickers hardness 7.5 GPa, ET300W manufactured by Ishihara Industry Co., Ltd.)
- Grinding media A4 Titer (average particle size 0.26 m, Vickers hardness 7.5 GPa, Ishihara Sangyo ET500W)
- Grinding media A5 Alumina (average particle size 0.5 m, Vickers hardness 15 GPa, high purity alumina AKP-20 manufactured by Sumitomo Chemical Co., Ltd.)
- Grinding media A6 Alumina (average particle size 0.75 ⁇ m, Vickers hardness 15 GPa, AKP-3000 manufactured by Sumitomo Chemical Co., Ltd.)
- Grinding media A7 Alumina (average particle size 2 ⁇ m, Vickers hardness 15 GPa, Sumitomo Chemical Co., Ltd. Sumiko Random)
- Grinding media A8 Alumina (average particle size 4.3 m, Vickers hardness 15 GPa, Sumitomo Chemical Co., Ltd. Sumiko Random)
- Grinding media A9 Alumina (average particle size 7 ⁇ m, Vickers hardness 15GPa, fine alumina AM-28 manufactured by Sumitomo Chemical Co., Ltd.)
- Grinding media A10 Alumina (average particle size 12 m, Vickers hardness 15 GPa, fine alumina AM-29 manufactured by Sumitomo Chemical Co., Ltd.)
- Grinding media Al 1 Alumina (average particle size 50 ⁇ m, Vickers hardness 15 GPa, A13 manufactured by Nippon Light Metal Co., Ltd.)
- Grinding media A12 Zircoa (average particle size 100 ⁇ m, Vickers hardness 12GPa, Torayserum manufactured by Toray Industries, Inc.)
- Grinding medium B1 Zircoyu (average particle size 100 ⁇ m, Vickers hardness 12GPa, Torayram manufactured by Toray Industries, Inc.)
- Grinding media B2 Zircoyu (average particle size 200 ⁇ m, Vickers hardness 12GPa, Torayram Co., Ltd., Torayserum)
- Grinding media B3 Zircoyu (average particle size 300 ⁇ m, Vickers hardness 12 GPa, Torayserum manufactured by Toray Industries, Inc.)
- Grinding media B4 Zircoyu (average particle size 500 ⁇ m, Vickers hardness 12 GPa, Torayram Co., Ltd.
- Grinding medium B5 Zircoyu (average particle size 800 ⁇ m, Vickers hardness 12GPa, Torayserum manufactured by Toray Industries, Inc.)
- Grinding media B6 Zirconia (average particle size 1000 ⁇ m, Vickers hardness 12 GPa, Torayserum manufactured by Toray Industries, Inc.)
- Grinding medium B7 Alumina (average particle size 2 111, Vickers hardness 15 GPa, Sumitomo Chemical Co., Ltd. Sumiko Random)
- Example 1 Based on the materials and ratios listed in Tables 1-5, the above grinding method was carried out.
- Comparative Example 1 the pulverization medium A was not added and only the pulverization medium B was used, and the other pulverization was performed in the same manner as in Example 3.
- Table 1 shows the change in the average particle size ratio of the grinding medium A to the average particle size of the material to be ground by changing the average particle size of the material to be ground.
- the average particle size ratio of the grinding media A to the average particle size of the material to be pulverized was changed by changing the average particle size of the grinding media B in Table 3 by changing the average particle size of the grinding media B in Table 3.
- Table 4 shows the change in the average particle size ratio of the grinding medium B to Table 1, and Table 4 shows the change in the volume ratio of the material to be ground and the grinding medium A. [0077] In the examples of V and misalignment, the average particle diameter of the obtained powder particles reached the target of 0.7 ⁇ m or less.
- a paste for an electron emission source for field emission was prepared as follows. As CNT
- Two-layer CNT (manufactured by Toray Industries, Inc.) was used. 100 parts by weight of CNT and 1000 parts by weight of the powdered glass particles obtained in Example 1 and 5 parts by weight of Solsperse 2400GR (manufactured by Abyssia) as a dispersant were weighed, and then a photosensitive polymer solution (methacrylic acid) as a photosensitive organic component.
- a photosensitive polymer solution methacrylic acid
- Acid monomer Z Methyl methacrylate monomer Z Styrene monomer 40Z40Z30 (Mole ratio) Copolymer of 0.4 equivalent of glycidyl metatalylate added to the carboxyl group (weight average molecular weight 43000, 2500 parts by weight of acid value 100) dissolved in 40% by weight of tervineol, 400 parts by weight of photosensitive monomer (tetrapropylene glycol dimetatalylate), photoinitiator IC369 (2 benzyl-2 dimethylamino-1— (4 morpholinophenol) butanone 1), manufactured by Ciba Specialty Chemicals) Add 400 parts by weight, knead with 3 rollers, Was a strike. To adjust the viscosity, 4000 parts by weight of terbinol, a solvent, was added.
- an electron-emitting device was produced as follows.
- a force sword electrode was formed by sputtering ITO on a glass substrate.
- the paste for an electron emission source obtained as described above was printed in a 50 mm square pattern by screen printing.
- UV exposure was performed from the top with an ultrahigh pressure mercury lamp with 50 mW Zcm 2 output.
- it was developed by applying a 1% by weight aqueous solution of sodium carbonate in a shower for 150 seconds, washed with water using a shower spray, and photocured to remove the portion.
- the pattern obtained here was heated in the atmosphere at a temperature of 450 ° C to obtain a CNT film.
- the CNT film was brushed with a tape having a peel adhesion strength of 0.5 NZ 20 mm.
- a phosphor was printed on a newly sputtered ITO glass substrate to produce an anode substrate. These two glass substrates were bonded with a 200 / zm gap film in between to obtain an electron-emitting device.
- a photosensitive insulating layer paste for field emission was prepared as follows.
- an insulating layer having an emitter hole with a diameter of 30 ⁇ m was manufactured as follows.
- a force sword electrode was formed by sputtering ITO on a glass substrate.
- the photosensitive insulating layer paste obtained as described above was solid-printed by screen printing so that the film thickness after drying was 20 / zm.
- UV exposure was performed with an ultrahigh pressure mercury lamp with 50 mWZcm 2 output from the top surface.
- a 0.01% by weight aqueous solution of sodium carbonate was developed by applying it for 150 seconds in a shower, washed with water using a shower spray, and photocured to remove the portion.
- the pattern obtained here was heated in the atmosphere at a temperature of 450 ° C. to obtain an insulating layer having an emitter hole with a diameter of 30 ⁇ m.
- the surface roughness Ra of the flat portion of the insulating layer was measured and found to be 0.01.
- An electron emission source paste and an electron emission device were prepared and evaluated in the same manner as in Example 25 except that the glass powder particles obtained in Example 1 were replaced with the glass fine particles obtained in Comparative Example 1. Two or more irregularities of 0.5 m or more were observed on the periphery of the pattern. In addition, when a voltage of 1 to 5 kV was supplied to the anode electrode of the electron-emitting device, phosphor emission due to electron emission obtained from CNTs was confirmed, but arc discharge that appears to be caused by irregularities in the pattern periphery occurred. ⁇ Comparative Example 8>
- the surface roughness Ra of the flat portion of the insulating layer was measured and found to be 0.3.
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Abstract
Description
Claims
Priority Applications (6)
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KR1020087014832A KR101390757B1 (ko) | 2006-02-27 | 2007-02-26 | 분쇄 매체를 사용하는 분말 입자의 제조 방법 |
JP2007511117A JP5309562B2 (ja) | 2006-02-27 | 2007-02-26 | 粉末粒子の製造方法、粉末粒子、組成物およびこれを用いるフィールドエミッションディスプレイ部材の製造方法 |
CN2007800066280A CN101389411B (zh) | 2006-02-27 | 2007-02-26 | 组合物及使用该组合物的显示器部件的制备方法 |
EP20070714897 EP1990095A1 (en) | 2006-02-27 | 2007-02-26 | Method for producing powder particle by using grinding medium |
US12/224,426 US8241418B2 (en) | 2006-02-27 | 2007-02-26 | Producing method of powder particles by using grinding medium |
US12/923,344 US8747545B2 (en) | 2006-02-27 | 2010-09-15 | Producing method of powder particles by using grinding medium |
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US12/224,426 A-371-Of-International US8241418B2 (en) | 2006-02-27 | 2007-02-26 | Producing method of powder particles by using grinding medium |
US12/923,344 Division US8747545B2 (en) | 2006-02-27 | 2010-09-15 | Producing method of powder particles by using grinding medium |
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US (2) | US8241418B2 (ja) |
EP (1) | EP1990095A1 (ja) |
JP (1) | JP5309562B2 (ja) |
KR (1) | KR101390757B1 (ja) |
CN (2) | CN101992141B (ja) |
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WO2008143189A1 (ja) * | 2007-05-18 | 2008-11-27 | Asahi Glass Company, Limited | ガラス微粒子集合体およびその製造方法 |
JP2010090003A (ja) * | 2008-10-09 | 2010-04-22 | Idemitsu Kosan Co Ltd | 硫化物系固体電解質の製造方法 |
JP2010111520A (ja) * | 2008-11-04 | 2010-05-20 | Nippon Electric Glass Co Ltd | ビスマス系ガラス粉末の製造方法 |
JP2013220982A (ja) * | 2012-04-19 | 2013-10-28 | Central Glass Co Ltd | ガラス粉末材料及び多孔質なガラス質膜の製造方法。 |
JP2013545878A (ja) * | 2010-12-13 | 2013-12-26 | サン ケミカル コーポレイション | ミリング媒体を顔料粒子分散中に可溶化する方法 |
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- 2007-02-26 CN CN2007800066280A patent/CN101389411B/zh not_active Expired - Fee Related
- 2007-02-26 WO PCT/JP2007/053465 patent/WO2007105466A1/ja active Application Filing
- 2007-02-26 KR KR1020087014832A patent/KR101390757B1/ko not_active IP Right Cessation
- 2007-02-26 TW TW96106404A patent/TWI393587B/zh not_active IP Right Cessation
- 2007-02-26 US US12/224,426 patent/US8241418B2/en not_active Expired - Fee Related
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JP2010111520A (ja) * | 2008-11-04 | 2010-05-20 | Nippon Electric Glass Co Ltd | ビスマス系ガラス粉末の製造方法 |
JP2013545878A (ja) * | 2010-12-13 | 2013-12-26 | サン ケミカル コーポレイション | ミリング媒体を顔料粒子分散中に可溶化する方法 |
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Also Published As
Publication number | Publication date |
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EP1990095A1 (en) | 2008-11-12 |
JPWO2007105466A1 (ja) | 2009-07-30 |
US8241418B2 (en) | 2012-08-14 |
CN101992141A (zh) | 2011-03-30 |
TWI393587B (zh) | 2013-04-21 |
CN101389411B (zh) | 2010-12-01 |
TW200800400A (en) | 2008-01-01 |
US8747545B2 (en) | 2014-06-10 |
KR101390757B1 (ko) | 2014-04-30 |
KR20080097393A (ko) | 2008-11-05 |
CN101389411A (zh) | 2009-03-18 |
US20110068202A1 (en) | 2011-03-24 |
JP5309562B2 (ja) | 2013-10-09 |
CN101992141B (zh) | 2015-07-01 |
US20090101737A1 (en) | 2009-04-23 |
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