TW552250B - Barium titanate dispersions - Google Patents

Abstract

The invention provides slurries, dispersions, or slips of barium titanate-based particles in a non-aqueous medium and methods of their production. The particles have a costing comprising a metal oxide, metal hydrous oxide, metal hydroxide or organic acid salt of a metal other than barium or titanium. At least 90 percent of the particles have a partible size less than 0.9 micrometer when the coated particles are dispersed by high shear mixing.

Description

552250 A7 V. Description of the invention (1) The present invention relates to the acid steel dispersion which is more particularly non-aqueous. Ϋ mtmm nnn ϋ ϋ ϋ n ϋ I · II (please read the note on the back first to write this page) ”acid lock dispersion Thing. The high permittivity of the material mainly composed of barium acid makes it multi-layered-line capacitors, generally referred to as " MLC, S_, including alternating layers of dielectric and conductive substances. Examples of MLC.s are disclosed in U.S. Patent Nos. 3 612 963 and 4,435,738. The silver, silver, silver alloy, copper, and aluminum are recorded as the conductive materials used in the two MLC, S. The dielectric layer of MLC is usually prepared from a high-temperature dispersion, and is known in the art such as " muddle ". Such muds typically contain a powdery substance that is predominantly osmotic acid, and a polymerized adhesive = j-based or non-aqueous solvent. A thin film of a binder-stabilized powder made by slurry casting or coating was dried to obtain a "green" layer of a ceramic dielectric. The green layer is coated with a conductive material in a pattern shape, and then stacked to obtain a thin laminated layer of green ceramics with two alternating currents and conductances. This stack was cut into paper. Size: Square body, heat it to burn off organic substances such as adhesives and dispersants. However, the particles of the substance mainly composed of barium acid are burned to form a dense, dense ceramic with the thinnest layer. Capacitance junction n junction temperature of the dielectric and conductive layers ^ Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs, j is about 1000. 〇 to 1500. 〇's range. The ceramic dielectric density is increased during sintering to achieve the result of particle fusion and strengthening to form particles. And using a particle growth inhibitor, the size of ceramic particles in the MLC dielectric layer will be larger. For example, it is 3 times larger than the original elementary particles. Moreover, not all porous parts are removed during the sintering process. Typically, about 2% and 10% of the porous portion will remain in the Mlc second dielectric layer. The shortcomings of these holes or holes in the dielectric layer will make larger particles: -4-This paper size applies to the Chinese National Standard (CNtS) a4 specification (2) 0x297 mm) 552250 A7 ---_____ B7 V. Description of the invention (2) The size of the ceramic appears larger. Some key capacitive properties, such as power-off voltage, DC leakage will be affected by the thickness of the dielectric, particle size, and shortcomings of the holes. As an example, it is believed that an effective dielectric layer requires many particle thicknesses, truthfully == 3 to 5 fewer particles thick. Because the defects in any MLC layer have a significant destructive effect on their performance, MLC, S is made of a thick enough dielectric layer to effectively reduce the impact of ceramic defects. This defect may be caused by arbitrary large particles or holes. Not good for MLC performance. Due to the market demand for miniaturization of electronic device designs, the industry of MLC needs to make it a thinner dielectric layer on ceramic materials without the tragic effect of large dielectric thickness particles and hole sizes. The barium titanate powder is prepared by a known method, such as an example calcination or hydrothermal method, which has large particles and / or strong agglomerated fine particles, and the size is substantially larger than the working micrometer. Such particles and agglomerates are not immediately ready to be processed and have fine-grained, ultra-thin dielectric layers, as in the example below 4.5 microns. Therefore, its representative technology should obtain barium titanate-based materials and dispersions-pre-prepared, and can be suitable for manufacturing MLC, s with thinner dielectric ceramic layers, such as examples below 4 microns, and Has acceptable or expected electrical properties, including DC leakage and power-off voltages, without the need for induced ball grinding. From the viewpoint, the present invention provides a polymer, dispersion, and slurry of particles mainly composed of barium titanate in a non-aqueous medium. The particles contain a coating film including metal oxides, metal hydrated oxides, metal hydroxides or non-selling or organic metal organic acid salts, wherein when the coated particles are mixed and dispersed with high shear force, at least 90% of The particles have a particle size of less than 0.9 microns. -5- This paper size is in accordance with Chinese National Standard (CNS) a4 specifications (21〇 (Please read the note on the back --- write this page). 297 mm printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs) 552250

V. Description of the invention (3) Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs with the other two coatings based on barium titanate " referred to as the coating film of barium titanate, barium titanate as an oxide, and Other oxides are mainly barium and titanate, and 彳 A ^, formula A AB03, where A represents one or more divalent metals such as barium, molybdenum, blood, 1 I, total zinc, and B represents one or more tetravalent metals such as', tin, zirconium and hafnium. :: Another: From a viewpoint, the present invention provides a slurry, dispersion, or method. The method includes mixing with high shear force and dispersing particles mainly composed of barium titanate in a non-aqueous medium. Until 90% of the particles have a particle size of less than 0.99, "i • Tochigi This particle has a coating film including metal oxides, hydrated oxides, metal hydroxides or non-barium Or titanium metal organic acid salts. From another perspective, the present invention provides another method for forming a slurry, dispersion, or slurry. This method involves hydrothermally forming a slurry of particles mainly composed of barium titanate in an aqueous medium. This method further includes forming a coating film on the particles, including metal oxides, metal hydrated oxides, -metal hydrogen emulsions, or non-barium or metal organic acid salts. Brief Description of the Figures Figures 1 A, 1 B 'and 1 C are specific examples of the barium titanate particles of the present invention. I particle control distribution diagram. After mixing for 4 to 5 minutes under high shear force, additional levels are used; After 30 minutes of mixing, and after 45 minutes of additional horizontal grinding and mixing; and Figures 2A 'and 2B are particle size distribution diagrams of another specific example of the barium acid particles of the present invention, at high shear After 10 minutes of force mixing and 30 minutes of high shear mixing. -6- This paper size applies to the Chinese National Standard (CNS) A4 specification (210 X 297 mm) — l · --- ^ -------- Package—— (Please read the precautions on the back first to write this Page) Order · • Line!

V 552250 Α7 Β7 Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs V. Description of the Invention (4) Other novel features and perspectives of the present invention will be explained in detail by the following invention, and the scope of the accompanying graphics and patent application will be made clearer. Detailed description of the invention The present invention is directed to a slurry, dispersion or slurry of particles mainly composed of barium titanate in a non-aqueous medium. This particle includes a coating film on at least a portion of the particle surface. The coating film includes a metal oxide, a metal hydrated oxide, a metal hydroxide, or a non-barium or metal organic acid salt, or a mixture thereof. The coated particles have a particle size of less than 0.9 microns under high shear dispersion. '' Particles based on barium titanate are dispersible and do not require sphere grinding as a sub-micron dispersion in a non-aqueous medium, which is manufactured] ^ 1 ^ (:, 3 advantages, this MLC's has a dielectric layer Contains sub-micron particle size and high power-off voltage. High-shear mixing effectively reduces the size of agglomerates of barium titanate-based particles, and includes deagglomeration or separation of aggregates into smaller coating film particles without Spherical grinding is required, which involves hitting particles with hard spherical grinding media such as rods, balls, or zirconia particles and the like. Because spheroid grinding may split particles into smaller than the basic particle size, resulting in non-uniform The particles expose an uncoated surface. In a preferred embodiment, the particles T of the present invention are not ground by a sphere, and the main part of the surface of the particles is covered with a coating film. In another aspect of the present invention, The unground particles are uniform or spherical. Particles based on barium titanate are useful in providing a single lithium capacitor, which includes a ceramic king body with a particle size below 0.3 micron. Better Mα, performance Capacitor temperature constant of X7R or Y5V, and the thickness of the dielectric. This paper is suitable for standard (CNS) A4 size ⑵Q χ tear (please read the precautions on the back first --- write this page) Order: • Line-552250 A7 B7 5. Description of the invention (5) Below 5 micrometers, and the dielectric strength is at least 50 volts per micrometer. The basic particle size of particles mainly composed of barium titanate can be measured by methods known to those skilled in the art. Examples of such methods are the use of scanning electron microscopy (SEM) or transmission electron microscopy (TEM). Although it is understood that particles mainly composed of barium titanate can contain elementary particles of various sizes, coating film particles mainly composed of barium titanate Have an average basic particle size of less than 0.6 microns, preferably the particles have a basic particle size of less than 0.5 microns; more preferably less than 0.4 microns; and even more preferably the particles have a basic particle size of less than 0.3 microns It is best for this particle to have a basic particle size of less than 0.2 micrometers. Particles based on "barium" may exist in shapes other than the basic particles, such as the example of a polymer of a basic particle, and / or agglomeration of the basic particles Solidified body.SEM And TEM are not effective in distinguishing the particle size distribution of elementary particles, aggregates of elementary particles, and solidified bodies of elementary particle aggregates. For example, the light scattering technique is used to distinguish the particle size of particles that are mainly barium acid. Method 'Suppose that the preparation of the analysis does not include processing, which will change the distribution of agglomerated or solidified particles, such as decoagulation due to ultrasound, high shear mixing, or grinding. One such automatic light scattering technique uses H 〇rIB a LA-910TM, light-scattering particle size analyzer or similar device. This analysis typically represents the volume fraction of elementary particles, the separation particle size of agglomerates and coagulates at ten times or one tenth, Normalized frequency. As used herein, the term "particle size" refers to individual particles in the powder, and may include elementary particles, aggregates of elementary particles, coagulated bodies of aggregates, and mixtures thereof. In one aspect of the present invention, at least 90% of the particles of "barium titanate" coated with metal oxides are dispersed in the particles mainly of barium titanate-8-This paper is in accordance with Chinese national standards (CNSM4 Specifications (210 x 297 mm) (Please read the note on the back --- write this page) -Line · Printed by the Employee Consumption Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 552250 V. Description of the invention (6) & Eight of the particle diameters are lower than 0.8 micron, preferably lower than 0.7 micron; the best is lower than G. 6 micron. In the better viewpoint of the present invention , At least the particles have a particle size of less than 0.05 micrometers in the barium acid powder; preferably less than 0.4 micrometers; and more preferably less than 0.3 micrometers. The characteristics of the grain knife cloth include D %, Which is a small particle size at one-tenth of the largest particle TI; D50 represents the centerline diameter, and D10 is the largest particle size among the ten blades of the smallest particle. The ratio of D90 / D10 is a suitable characteristic, It is used to discern the width of the age-diameter distribution curve. It has a ratio of less than 4. More preferably, the ratio of D9o / D10 is less than 3; more preferably, the ratio of the core is less than 25. ", as used in the present invention " dispersion " A two-phase system in which solid particles are suspended in a non-aqueous medium. In a preferred embodiment, the stability of the dispersion or the resistance to sedimentation of suspended solid particles can be increased by the use of a dispersant. Except where the text clearly states otherwise, the metal Oxide only means that the term "metal oxide" as used herein is used to describe coatings of metal oxides, metal hydrated oxides, metal hydroxides, and organic acid salts of metals. Organic acid salts can be converted to oxides or hydroxides, as in the example by thermal decomposition, which occurs when the ceramic adhesive is burned out and / or the ceramic is sintered and heated. As used herein, "mixing to shear" , Means mixing in a liquid medium to give the solidified body of the coating film particles sufficient energy to separate into smaller particles, and there are no solid tool impacts, such as rods, cylinders, or hard spheres such as dioxide Hammer ball Hard media is suitable for some high-altitude shear mixing. The paper size is applicable to China National Standard (CNS) A4 (210 x 297 mm).

I! Sang (please read the note on the back fmjc first to write this page) | &.; -Line-552250 A7 B7 V. Description of the invention (in the stone equipment, and the small-sized medium is used to generate shear force and There is no impact force. Although high shear mixing can be performed by various types of equipment as described below — lh ----------- M i — f Please read the note on the back first? (Write this page) Scenery> It is difficult to accurately divide the size of this force under high shear forces to separate the solidified body. • Line-Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs as defined above "mainly barium acid, with reference to" barium acid ", which has additional metal oxide coatings, and others based on barium and titanic acid Salt-based oxides' have the structure AB03, where A represents one or more divalent metals such as lock, bow, lead, gill, magnesium, and zinc, and B represents one or more tetravalent metals such as, Tin, zirconium, and zinc. A preferred barium titanate-based material is typically used in Y5V applications. It has the structure Ba (1-x) Ax〇. But hi-wByO2, where X and y can be 0 and 1. Integer, where a represents one or more non-barium monovalent metals such as er, wa, or wei, and B represents one or more non-chin tetravalent metals such as tin, germanium, and thorium. Where other metals represent impurities, X and y are small, such as when the example is less than 0. In other examples, other genera or metals can be used to provide a significantly calibrable compound, such as barium acid bow, barium titanate-gill, titanate -Barium hammerate, and the like. In other examples, X and y are 丨, barium or titanium can be Its appropriate valence metal substitution 'to obtain compounds such as lead titanate or barium hammerate. There are also other examples where the compound can have multiple partial substitutions of barium or titanium. Examples of such multiple partial substitution compositions are as follows Expression

Ba (1m,) PbxCax, Srx " CUTi (1.yy, y ") SnyZiyHfy" 〇2 where X, X ', X ", y, y ·, y ·, each of which is 2 0, and (χ + χ , + Χ ") ^, and (y + y, + y ") < l. In many cases, the material mainly containing barium titanate will be treated with per0vskite structure, and it is preferred that the barium titanate material has per〇vskite -10- This paper standard is applicable to Chinese National Standard (CNS) A4 regulations) --- -552250 A7 B7 V. Description of the invention (8) Structure. When the barium titanate particles produced by the hydrothermal method are dried into a powder in a conventional manner, the particles form a strong solidified particle, which cannot be effectively mixed with a simple Amano force to de-solidify. The dispersion made from this dry, solidified barium titanate-based particles has a submicron basic particle size that requires substantially longer time to impact and grind to obtain particles around the micron tube, which are longer Sub-micron particles were obtained by deep grinding. In contrast, solidified barium titanate-containing particles with a metal oxide coating film have a sub-micron basic particle size, and can be mixed with a slurry containing such particles in an aqueous medium by a moderately acting high shear force. Materials, dispersions, or slurries to de-solidify them into coating film particles in the sub-micron size range. The non-aqueous slurry, dispersion, or slurry of the barium acid-based particles of the present invention can be prepared from barium titanate-based particles, which are produced by a hydrothermal method and maintained in an aqueous environment. The water-based slurry is at least until the particles are coated, and then the water phase is replaced by a non-aqueous phase as described further below. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs ϋ tr I n ϋ «ϋ ϋ -ϋ ϋ H ϋ II ·. ^ 1 ^ 1 (please read the note on the back ^^ write this page first) — the submicron slurry of barium titanate-based particles can be prepared by hydrothermal method. Nos. 4,832,939, 4,829, 3, and 4 '8 6 3, 8 3 3 are disclosed. In this hydrothermal method, an excess of about 200 mol / o of barium hydroxide solution is typically added to the hydrated oxidized slurry and heated, often to a temperature of about 10 (rc and In the range of 20.0%, to obtain submicron particles with per0vskite crystalline structure. This particle size and particle size distribution can be adjusted by controlling changes in various methods, such as slurry and; i liquid Temperature, the addition rate, and the rate of heating to the temperature at which per0vskite is formed, and the cooling rate at the temperature formed by per0vskite. -11-This paper size applies to the Chinese national standard (CNSM4 specification (210 x 297 mm)) 552250 A7

Please read the note on the back first b Write the page of this book; Ding 4 552250 A7 B7 V. Description of the invention (1〇) ___r___W___I IIII · II (Please read the note on the back first to write this page) Oxide, hydroxide or organic Acid salt layer. If the metal has a higher dissolution rate, such as cobalt and nickel, the oxide coating becomes more difficult to use and maintains no longer dissolving. Therefore, it is generally preferred to use these more soluble metal oxide coatings as topcoats on the more easily deposited metal oxide layers. The alkaline environment also minimizes the dissolution of barium, and particles with a barium-free and thorium-free coating can be obtained immediately. Particle coatings to be used in ceramic capacitor applications typically have a thickness of less than 10% of the particle diameter, typically less than 20 μm thick 'and preferably no more than 5 nm and 10 nm Between the thickness. -Line- Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs Useful organic acid salt coatings include metal organic acid salts with a low dissolution rate. Examples of such organic acid salt coating films are metal salts of oxalic acid, citric acid, tartaric acid, and palmitic acid (for example, niobium oxalate). It is believed that the organic acid salt will be converted into a metal oxide when the adhesive is burned off. The choice of metal is based on the enhancement of processing or properties to be imparted to the MLC's. The metal in the coating film is typically selected from the group consisting of ytterbium, lithium, magnesium, calcium, gills, hafnium, zirconium, hafnium, vanadium, niobium, thorium, tungsten, manganese, nickel, boron, silicon, antimony, tin ' Yttrium, steel, lead, and steel rare earth elements. It is preferably “acid-locked particles” which do not originally have barium and hafnium metal oxide coatings. When ceramic capacitors need to have hungry: electrical properties, it is useful to provide “barium acid particles with dopants, such as oxide, hafnium oxide, or a combination of neodymium oxide and nickel oxide, or cobalt oxide ... To provide ceramic capacitors When sintering at a relatively low temperature, as in the example == 00 C and 120,000. (: The range is compared to the range of about 130 (rc and 160th generation), which provides barium osmate particles containing dopants, which can promote low-temperature firing. Such low-temperature sintering aids include oxides and zinc oxides , Zinc borate, rhetoric, ..., and combinations thereof. Dielectric improvement and sintering temperature

This paper size _ + Guan Jiaxian (CNS) A4 secret G -13-552250 V. Description of the invention (1), metal oxides can be effectively washed after particles and in the formation of separable & Among the particles that are mainly locked, the consumer cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs printed on the particles that are based on barium titanate produced by hydrothermal method, the slurry can be washed, and the slurry has a water content It can be lowered to obtain concentrated slurry, cake or powder. Moreover, the slurry, wet cake or powder can be treated with dispersant to obtain dispersion, and further, the adhesive and other additives can be used to obtain slurry. It is preferred to remove water from the plutonium to avoid or at least minimize the formation of strong particles, such as during calcination. Some metal oxide coatings may remain as hydrated metal oxides due to their constant burning or drying. Form, if P η is not maintained close to the minimum solubility of the metal oxide, it may dissolve. For example, if ρΗ is not maintained close to work 0, nickel oxide or oxide will become somewhat dissolved. Therefore Maintaining proper coating film particles, the pH of the aqueous component is preferably maintained in the range of 9 to 丨 丨. Metal oxides are coated with barium titanate-based slurries, which are easy to manufacture with a small amount of solids. Such as the example of 30% by weight of barium titanate-based particles. Higher solid content is often better used to make MLC, s. Therefore, if the slurry of the present invention is used to directly make MLC, s, then It is useful to concentrate the slurry, such as by removing water by filtration to at least 40% by weight of solids; preferably at least 50% by weight of 0/0 solids; more preferably at least 5 $% by weight of solids; And still more preferably at least about 60 to 75% by weight of solids. Dispersants and adhesives can be added to the concentrated slurry to obtain a slurry or stable dispersion of particles mainly composed of barium titanate. As mentioned above, After the barium titanate-based particles are coated, the water phase can be replaced by the water phase. The water phase can be exchanged with the organic liquid phase by solvent exchange or steaming. 21G X 297 public love) ~ 552250 A7 B7 V. Description of the invention (12) Generation. IU .--- ^ -------- installation can be used in this method. (Please read the notes on the back ^ write this page first) It consists of a flat pan inside, which is connected to the central water storage tower. The liquid flows through F and Pm, and is removed by the middle water tower.-Once, the cake is separated by centrifugal force to leave the plate. This solid = reflow = valve From the middle to the next processing step, it is considered that the omentum material is used due to the hydrothermal hydrazine-locked secondary micron particle size. • Line. When operating the solvent exchange method, it is first related to the fact that the aqueous solution of the cyanate-locked particles is not taken. The water is removed through the ultrafiltration membrane. After removing most of the water, an anhydrous water-miscible organic solvent such as methyl ethyl ketone (MEK) or toluene (as described below) is injected into the filter device. The water-miscible solvent is added and then removed by the filtration device through the ultrafiltration membrane material until the hydration amount of the barium titanate filter cake is reduced to the required amount. Once water is removed from the filter cake using a water-soluble solvent, a water-insoluble solvent is added. After adding sufficient water-insoluble solvent through the ultrafiltration material and removing it, the concentration of the water-soluble solvent is diluted to the required amount. Separate the barium titanate from the ultrafiltration material and place it into a mixing tank located under the filter. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs Once “into the mixing tank located under the mixing device, the dispersant is added thereto, and then the contents of the container are mixed until a homogeneous slurry is obtained. If a low water content is required, a desiccant such as activated aluminum can be added. Disperse the slurry and remove it for grinding and packaging. Another method to complete the solvent exchange is via the steam room method. This method involves mixing batch distillation vessels, condensing heat exchangers, and phase separation tanks. During operation, the aqueous barium titanate slurry is pumped into the distillation tank, and then added to the 15- this paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 552250 A7 B7 V. Description of the invention ( 13) Employees of the Intellectual Property Bureau of the Ministry of Economic Affairs consume organic solvents printed by cooperatives. If the desired organic solvent is not miscible with water, a small amount of a water-miscible solvent such as a high molecular weight alcohol may be added. This ingredient is remixed 1 and emulsified and heated. The distillation method preferably uses a high molecular weight solvent, which has a higher boiling point than water. Heating the mixture selectively drives off water and separates it from the barium titanate dispersed in the organic medium. The phase separation tank is located downstream of the condensation unit and separates water from any solvent, which can also be removed during distillation. The solvent is then pumped back into the distillation vessel and the water is pumped off. It is also possible to use inscriptions in phase separation, so that steaming occurs at lower temperatures. A dispersant can be added in the steam room method to prevent the slurry from solidifying in the distillation vessel. Once the desired water content is reached, the solvent is not recycled and the mixture is then concentrated by distillation to the desired percentage of solids. Similar to the ultrafiltration method described above, if a low water content is required, the mixture can be introduced into the distillation tank via a bed containing a desiccant, such as activated silica, or activated silica. It should be noted that the thermodynamic efficiency of the distillation method can be improved by adding the upstream barium titanate slurry and feeding the aqueous barium titanate slurry into the distillation vessel. These ultrafiltration modules remove most of the water from the aqueous barium titanate slurry before they are introduced into the distillation process. The non-aqueous slurry can also be concentrated. For example, the solid cake obtained by filtration is a non-flowing solid containing a metal oxide coating film, particles and liquid mainly composed of barium acid. The non-aqueous wet cake may contain about 60% by weight of a solid mixed non-aqueous solution in a solid state. More preferably, the cake may contain up to 65% by weight solids; and even more preferably at least 70% by weight solids. The cake may contain up to 85% by weight of solids. In non-aqueous wet cakes, the non-aqueous solution should have a p Η 値 greater than 8 to suppress the dissolution of metals. Better -16- This paper size is in accordance with Chinese National Standard (CNS) A4 (2〗 〇χ 297mm) '' --- (Please read the precautions on the back first and write this page) Order:- Line-552250 Printed by A7, Consumer Cooperatives, Intellectual Property Bureau of the Ministry of Economic Affairs. 5. Description of the invention (14) Γ: The range is between Γ8 and 12; more preferably, pH 値 is about 9 and "Fan '," barium sheet The predominant particle wet cake is a precursor to colloidal dispersions. 13 levels can be dispersed as an example by mixing with a dispersant. May be needed if needed-add additional liquid medium to transform the cake from a solid 'base to a fluid dispersion. At least in the case of non-aqueous wet cakes, the particles in the cake will become weakly coagulated for a while. The content of the liquid to maintain the cake is at least 15% by weight; more preferably, the liquid content of the cake is at least 20% by weight. % Is still more preferred as long as the cake maintains a liquid content of at least 25% by weight. Banjadi cakes are encapsulated in moisture barriers to suppress the loss of water content, which may promote the formation of strongly solidified particles, but not immediately solidify. Such radon barriers, such as polyethylene bags or polyethylene-coated fiber drums, can provide extended shelf time of at least one day or longer; preferably extended shelf time of at least 3 days; more preferably extended shelf time The time period is at least 30 days; the best time is to extend the shelf time to at least 90 days. This feature facilitates & storage and transportation of wet cake examples of the present invention. By knowing that the dispersant is added to the genus f, without the need to add liquid significantly, the clear cake is immediately converted into a liquid dispersion. Although the fluid can be added to the cake, 'the amount of dispersant required to convert the solid cake into a fluid dispersion is unusually small', as in the example, the weight of the barium acid-based material is typically less than 2% by weight f%. In some cases, no additional dispersant fluid volume is required to change > Wafer Microfluidic Dispersions. Desirable dispersants are polyelectrolytes, which include polyacid polymers such as polystyrene sulfonic acid and polyacrylic acid; cationic functionalized polymers include polyimide, such as polyetherimide and polyethylene- 17- 'Paper size applies to China National Standard (CNS) A4 specifications (2) 0 297 mm — ----------- installed. II (Please read the note on the back to write this page) Order : -Line! 552250 V. Description of the invention (15) Pyridamine. Polypropionic acid is better in many applications. Although polyacids can be shellfished, it is preferred that the acid groups have relative cations + + or other Metal dissolves, for example, it may be present: in the second film. The preferred cation in capacitor applications is -isolated. In some examples, it is suitable to use the impurity metal as the opposite cation for the polyacid dispersant. Regardless of the dispersant chosen, the appropriate amount of dispersant can be determined by titration methods known to those skilled in the art. When the amount of :: dispersant provides the lowest viscosity of the dispersant, the wave length of the dispersant used Can be reduced, such as by dilution or interaction with additives, The viscosity is increased to an unsuitable high viscosity. Therefore, in many applications, the use of a dispersant " minimum viscosity " is appropriate. A colloidal dispersion uses a better dispersant for capacitor applications The above 2 tests have been found to be ammonified polyfluoric acid, which has an average number molecular weight of about 8000. As an example, 0.75 wt% (40 wt% aqueous solution) of such ammonized polyacrylic acid has been found to transform wet cakes. It is useful for liquid dispersions. The dispersant can be added by convenient methods, such as mechanically dispersing the dispersant in the wet cake. When mixing with high shear force, the excess dispersant is replaced by the surface of the new particles. The area is consumed by the decoagulation method. Therefore, a large amount of dispersant can be easily added during high shear mixing. Distinguish wet cake from slurry, dispersion, slurry, and dry powder. Non-flowing solids, while slurries, dispersions, and slurries are fluid: solids, and dry powders are fluid solids. Wet powders may or may not flow depending on the liquid content. When more liquid When the body is removed, the Cheng powder gradually needs to be drier. However, it is important to note that the dry powder does not have to be completely dehydrated. Spray 18- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm). — (Please first Read the notes on the back to write this page) Order · 丨 Line 'Printed by the Consumers ’Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 552250 A7 B7 V. Description of the invention (16) Fog drying, freeze drying and low temperature air drying are used to obtain the coating film. Dry powder of barium titanate-based particles is preferred, and it remains dispersible, as long as it is mixed into a solution containing a dispersant, such as high shear mixing in the example. Therefore, the coating film is barium titanate The dry powder of the main particles is surprisingly dispersed in the dispersion of sub-micron particles without the need for continuous impact milling for a long time. Unlike known substances, it does not require high-energy grinding for many hours to reduce the particle size to a point shape, and the dispersion or slurry of the barium titanate-based particles of its coating film can be used to produce fine particles , Thin dielectric layer and capacitor with high power-off voltage. Printed by the Consumer Cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs I J ------------ Package --- (Please read the notes on the back to write this page) • Another aspect of the invention is, Provide sub-micron coating film dispersion of particles mainly composed of barium titanate in solution, by decoagulation of large dispersion (greater than 1 micron), weakly solidified metal oxide coating film with barium titanate The main particles are until all the particles are substantially less than 1 micron. In the preferred method of the present invention, a high solid dispersion containing particles between about 30% and 75% by weight is mixed with a high shear force dispersant. The optimal time for high shear-force mixing is measured experimentally using standard procedures. High-shear mixing can be effective in centrifugal extraction and solidification grinding, and is commercially available as an example, available from Silverson Machine Inc, (East Longmeadow, MA). Other devices useful for providing decoagulated dispersions include what are known as supergrinding, colloidal milling, and cavitation milling. A super-grinding grinding chamber containing a filling medium, which has a high-speed turntable on a central axis, and is commercially available, as in the example by Premier Mill (Reading, PA). Colloid grinding contains grinding grooves between the extension surface of the high-speed rotor and the holder, and is also available on the market, for example, available from Premier Mill. In cavitation grinding, it is on the market -19- This paper size is applicable to Chinese National Standard (CNS) A4 (210x297 mm) 552250 Α7 Β7 i, description of the invention (17) can be used 'as an example by Arde Barinco Inc. (Norwood, NJ) is available. The fluid is withdrawn through a series of rapid opening and closing chambers, which rapidly compress and decompress the fluid 'to give a high frequency shear effect, which can de-solidify the particles. It is expected that concentrated pastes, dispersions, wet cakes, wet powders, or dry powders will work equally well for manufacturing high performance capacitors, depending on the particular capacitor manufacturing equipment or method. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs to determine the amount of effective dispersant, which is used for weakly solidified coatings mainly containing barium acetate, including the use of high shear mixers such as Silverson Model L4R A 500 g sample of the dispersion was mixed with a high shear force, which contained 70% by weight of coating film particles in an alkaline non-aqueous solution at a temperature range between 25.0 and 3 (TC, pH 値 in When the coating film does not dissolve, and contains an effective amount of dispersant, it will solidify the coating film particles in an effective time. The effective amount of dispersant is sufficient to maintain the separated coagulum and agglomerates to a smaller particle size, and Will not solidify again. The effective amount of dispersant will change, depending on the size, particle size, coating film and dispersant powder characteristics. Effective amount of dispersant and effective time can be observed by those skilled in the art, observe Effective variables, such as dispersant concentration and high shear mixing time, are measured immediately with fewer standard procedures to reduce the size of the particle size distribution. The effective amount of these variables will make the particle size analysis response high shear Shear Mix The effect of deconsolidation. For many examples, it has been found that an effective amount of ammonium polyacrylic acid dispersant (number average molecular weight is about 8000) is about 1 weight per particle and dispersant total ❶ / 〇 Dispersant, and effective high-shear mixing time is about 1 minute. Σ The main particles of the barium titanate of the coating film are prepared by the hydrothermal method substantially -20- 552250 A7 B7 V. Description of the invention ( 1S) Spherical and homogeneous in appearance. Such particles remain substantially spherical, even after reducing their size with high shear mixing. Occasionally, spherical particles may be paired The generation of paired particles is quite rare. Using spherical particles compared with non-spherical ground powders, the powder characteristics are expected to have a high surface area with a bet surface area of at least about 4 m 2 / g; preferably Sphere particles have a bet surface area of at least about 8 m / g '. Better earth-like particles have a BET surface area of at least about 2 m2 / g. Sub-micron coatings of barium titanate particles are compatible with a wide variety of substrates. Agents, dispersants, and releases The agent is suspended, which uses a non-aqueous solvent to obtain the slurry of porcelain casting. The particles mainly composed of barium titanate are dispersed in a solution containing a dissolved polymerization adhesive, and optionally other dissolved substances, such as plasticizers, release agents , Dispersant, release agent, anti-blocking agent and wetting agent. Useful organic solvents have low boiling points and include benzene, methyl ethyl ketone, acetone, dibenzobenzene, methanol, ethanol, propanol, 1,1,1-di Ethyl chloride, tetrachloroethylene, pentyl acetate '2,2,4-diethylpentanediol monoisobutyrate, toluene, digas, rosin, ethanol, bromochloromethane, butanol, ethyl Acetone, methyltributyl ketone, cyclohexyl &, methanol, n-propanol, isopropanol, n-butanol, n-octanol, benzyl alcohol, glycerol, ethylene glycol, benzyl, propionic acid, n-propanol Caprylic acid, ethyl acetate, butyric acid butyrate, n-hexane, and the like, including herba compound, and a mixture with water such as a methanol / water mixture. In addition, many boiling organic acid solvent mixtures have a low point of 1 m 1 /, ′ low, and can be used as a carrier. The solvent mixture can include, for example, 72% trichloroethylene m% ethanol, _A 'paper size applicable to China's national standard (Ci \ S) A4 specifications (21〇 (Please read the precautions on the back --- write This page) .Online! Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs -21-552250 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs A7 B7 V. Description of the invention (19) Ethyl ketone / 34% ethanol, 70% methyl ethyl ketone / 30% ethanol, 59% methyl ethyl ketone / 41% ethanol, 50% methyl ethyl ketone / 50% ethanol, 80% toluene / 20% ethanol, 80% toluene / 20% ethanol, 70% toluene / 30% ethanol, 60% toluene / 40% Ethanol, 70% isopropanol / 30% methyl ethyl ketone, 40% methyl ethyl ketone / 60% ethanol, and mixtures thereof. Except as disclosed above, the dispersant (anti-coagulant / humectant) is in a submicron, metal oxide coating. Useful in non-aqueous dispersions of barium titanate particles, including, for example, phosphates, glyceryl trioleate, ethoxylates, 2-amino-2-methyl_1-propanol, tall oil Hydroxyethylimidazoline, fatty acids such as glyceryl trioleate, lanolin fatty acid, poly (ethylammonium butyraldehyde), bis (tridecyl) sulfosuccinate Sodium peroxosulfate, sodium diisobutylsulfosuccinate, sodium dioctylsulfosuccinate, ethoxylated alkylguanamine, dihexylsulfosulfuric acid steel, sodium monoisobutylsulfosuccinate, benzoic acid , Oil-soluble horizontal acid g, poly (ethylene glycol) alkyl ether, oleic acid ethoxylate adduct, sorbitan trioleate, ethanoate stearate ethoxylate adduct, alkylaryl polyether alcohol Type, poly (ethylene glycol) ethyl ether, ethyl phenyl glycol, polyoxyethylene acetate, polyoxyethyl acetate, and the like. Preferred dispersants for organic solvent suspensions and slurries. Herring oil, corn oil, polyethyleneimine, and ammonium polyacrylic acid dimerized adhesive materials are useful in non-aqueous slurries such as examples, poly (ethyl #butyl butyraldehyde), poly (ethyl ethyl acetate) Vinegar), poly (ethylene glycol), cellulose polymers such as methylcellulose, ethylcellulose, samethylene fiber ^, methylcellulose, cellulose acetate Nitrile fiber: Polypropylene, Polyethylenimide, Lithium ketone polymer such as poly (methyllithium oxanthion) and M methylphenyl sintered oxygen), poly Styrene, Ding ## / Styrene ugly gathering ---------------- (Please read the note on the back first to write this page) · Line! National Standard (CNS) A4 Specifications_ -22- (210 x 297)

552250 V. Description of the invention (2 ()), poly (Ethyl ethene, p ratio, P, P, I), Department. / Check # servant name, Yongshang amine song, polyethers, poly , And acrylic polymers such as Gine, Yong (methyl acrylate), poly (methyl methacrylate), poly (methyl methacrylate), and copolymers such as ethyl methacrylate and propylene Copolymers of methyl gallate, poly (ethylene glycol), poly (acetylene alcohol), vinyl chloride acetate, _ · v τ I date ethylene), and the like. Polymerized adhesives are often useful as About 5 $ 9 〇 Tongue I 〇 / 口 口 Θ 〇: > soil 2 〇 weight I%. The best polymer available on the market is ACRYL0IDTM r 7 extension; ^ take people h ^ propyl I Ester polymer

Rohm & Haas Co.,). Oftentimes the organic medium also contains a small amount of plasticizer to reduce the glass transition temperature (Tg) of the polymer of the adhesive. The choice of plasticizer is basically determined by the polymer, which must be modified and can include phthalates (and mixed phthalates) such as dimethyl phthalate, diethyl phthalate , Dibutyl phthalate, dioctyl phthalate, butyl phthalate, phenyl phthalate, phosphoric acid ester, poly (alkenyl glycol), polyethylene glycol, glycerin, poly (ethylene oxide), hydroxyl Ethylated alkylphenols, dialkyldithiophosphonates, poly (isobutylene), butyl stearate, methyl rosinate, tricresyl phosphate, dipropyl glycol dibenzoate Acid esters, and their analogs. In a specific example, the organic solvent-based slurry of the present invention contains, per 100 parts by weight of the barium acid-based particles, 25 to 40 parts of an organic solvent, 2 to 5 parts of a dispersant, 5 to 20 parts of a polymerization adhesive, and 0 to 15 parts of a plasticizer. -23- This paper size is in accordance with China National Standard (CNS) A4 (210 X 297 mm) n I ϋ ϋ-in ϋ— ϋ iMmmm nn · · ϋ I · 1 · tam (Please read the notes on the back first Λ? Write this page) Order. · 'Line. Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs 552250

Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs

The particles mainly composed of manganese acetic acid are used in various non-aqueous tinctures, such as coupling agents; a wide range of mixtures in particles, providing: seed formula :: =: 垸 偶: choice of carrier . Hydrothermally-derived osmium acid locks are not only useful for rhenium powders, but also for particles / liquids. Although the silane coupling agent's surface is preferred, the coupling agent is preferably two: dry, or undried powder. Table 4 The horse is used to dry the particles after the foot to help and disperse in the carrier medium. And the dried eight-A porous beds have a simple mechanism to measure: the second achieves redundant coating, which is made by dispersing the processed powder in Y. The uncoated or partially coated powder will be partially or completely dispersed in water ' A while the fully coated particles, i.e. the stirrer, will still float on the water surface. Granules can be coated on one carrier medium and then transferred to another carrier medium by solvent exchange treatment (as described above), or by distillation. Although the silane coupling agent can be used on the powder surface before or after the solvent exchange, it is preferably used after the solvent exchange treatment. Silane coupling agents can be attached to the surface of the particles to help disperse in the required carrier medium, and to help the surface of the particles not to react easily. Organosilanes have the general formula RnSiX + w and exhibit two functionalities. χ is about the reaction with an inorganic substrate. The bond between X and the silicon atom by a coupling agent is replaced by the bond between the inorganic substrate and the silicon atom. X is a hydrolyzable radical. Figure 'is typically an alkoxy group, typically an alkoxy group, a fluorenyloxy group, an amine, or fluorine. The common alkoxy groups are methoxy and ethoxy groups, which can be obtained as by-products of methanol and ethanol when the coupling is reversed. Because gas-based stone sintering produces by-products of hydrogenated gas during the coupling reaction, it is generally less used than oxy-stone sintering. R -24-

(Please read the back: ^ 意 事 装 ·! Write this page} Order: 丨 Line · 552250

The Ministry of Economic Affairs and Intellectual Property Office is a non-hydrolyzable organic root, which can have a functional group that allows the coupling agent to bond with organic resins and polymers. The most widely used organosilanes have an organic substituent. Silanes in most particles are hydrolyzed before surface treatment. After hydrolysis, it is a form of reactive silanol, which can be condensed with other silanols. For example, these form silanol bonds on the surface of the silica filler. The stable condensation products also form with other oxides, such as aluminum, cone, tin, tin, zinc, and nickel. Less stable bonds are formed with oxides of boron, iron, and carbon. Experiential metal oxides and carbonates do not form stable bonds with si-O-. Water for hydrolysis can be obtained from many sources. It may be added, may be contained on the surface of the substrate, or may come from the atmosphere. The four steps involved in these silane reactions are illustrated below. 1. Initially three X radicals attached to silicon may undergo hydrolysis.

RSi (OMe) 3 + 3H20 RSi (OH) 3 + 3MeOH 2 · Then condensed to an oligomer: ·

R R R 3RSi (OH) 3-HO-Si-O-Si-O-Si-OH + 2H20

I I I

OH OH OH The oligomer is connected to the OH group of the substrate by hydrogen bonding ------------- install --- (Please read the note on the back first to write this page) Order: • f Printed by Consumer Cooperatives -25- This paper size applies to China National Standard (CNS) A4 (210 X 297 mm) 552250 A7 V. Description of the invention (23) f Jiu P, Shui (, Θ 咖啡 吹 1ί · 〇j丨 仰 * I · I [OK 〇Η · 〇κ

^ R K Κ · 0 — ¥ —〇 — Si —o- ^ si — OK + 2HP

(Please read the notes on the back first. 4 · Finally, a covalent connection with the substrate is formed when the dry H is hardened. The loss of water. Loss of water. With

K

R ^ write this page) Install OK OH OW,

• H0 —Si — O — Si—0- > Si—〇KIII Λ Λ 八 Κ Η Κ. Κ Η Κ VV V —ί _-!-! Substrate · απ · 4 · 2 0iJ—υ "; · 二0Η + 加 〇ί ί * Lh ία At the interface, there are usually only one bond on the surface of n substrates judged by organic money. The two remaining oxofluorenyl groups are either bonded to Shi Xi atoms of other coupling agents, or they are in a free state. Based on the methods known to those skilled in the art, green narrow bands with mud based on organic solvents can be formed on the surface of the carrier. See, for example, JC's intestinal line recommended in the testis paper of the sum technology of Academic Press (1976), Vol. 9, p. 197, and U.S. Patent Nos. 3,717,487 and 4,640,905, both of which And here for reference. In addition, there is a technical change in the ceramic materials used to convert mud into thin films and green layers of chicory. It is believed that the dispersion of the present invention will be found with less change

-lu ° J-丨 line · Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs -26- 552250 A7, the application method of Invention Note (24), such as the example of writing 4 lectures, two follow ,,, touch ★ & μRabbit Choosing a better floating medium and adhesive, diluting to the desired fluid viscosity, etc., Zuo Jiudou a * Human Λ various ceramic methods for manufacturing dielectric layers for MLC, s. Mud can be formed in the goods π + formed in the diaphragm, by spraying, by waterfall or casting (such as doctor's scalpel, shaper

) Forming a thin layer on a moving sheet, as well as the methods used by the MLC industry. After a long enough long non-aqueous liquid is removed from the film, a solid "road" " π 4 < 7 U cylinder green "film is obtained, which can be applied to materials with electrical materials or conductive materials. One or both sides of the previously aligned pattern of the substrate, such as ink, contains fine particles of palladium, nickel, nickel or palladium and silver alloys. The green film sheets are typically stacked, as examples are as high as or more, and are cut into MLC-sized cubes, which are ignited to burn off the polymerized adhesive and dispersant, and sintered to form a compact multilayer capacitor structure with Fine-grained dielectric layer. Conductive metals are used to form MLC between terminals that can be connected to alternate conductive layers. The unique particle size property of the particles mainly composed of barium titanate of the present invention is expected to produce novel MLC's having submicron particles & ultra-thin dielectric ceramics. Such a dielectric material should be suitable for a capacitance I with a large increase in volume. It is also expected that MLC's has an unexpectedly high power-off voltage. The absence of large particles, such as examples larger than 1 micron, should allow commercial manufacturing to have high yields, such as MLC with examples larger than 98/0, s containing multiple layers of dielectric such as 40 layers in the example. The particles of the present invention are expected to be preferably used for manufacturing dielectric ceramic layers MLC, s having a maximum particle size of 0.9 microns or less; more preferably, the largest particle size is less than 0.8 microns; most preferably The particle size is 0.7 microns or less. Another aspect of the present invention provides an X7R or Y5V capacitor, which has a dielectric structure sintered with a ceramic structure containing more than 20 layers mainly of barium octylate. -27 This paper size applies to China National Standard (CNS) A4 specification (210 x 297 mm) —ί ------------ install --- (please read the precautions on the back to write this page} ΊΟΙ, · ·-Line · Staff of Intellectual Property Bureau, Ministry of Economic Affairs Printed by the consumer cooperative 552250 A7 B7 V. Description of the invention (25) Where the layer is less than 5 microns thick, as in the example 2 to 4 microns thick. More dielectric layers such as examples 250 or 500 may be better, depending on the MLC Depending on the design. Thin dielectric layers allow MLC, S to increase the number of dielectric layers for standard size MLC or MLC's contain a fixed number of layers to fit smaller size packages. The result is a standard size MLC package The electrostatic capacity can be increased immediately by 5 to 10 times or more. In order to provide a single X7RMLCW particles, the dielectric should be better coated with niobium, #, nickel and manganese oxides. For low fire capacity, For example, when the sintering is below 1200 ° C, the preferred metal oxide coating film may also contain an oxidation grade. An ultra-thin dielectric layer with a thickness of less than 4 micrometers is obtained, preferably the particles contain a basic particle size of less than 0.3 micrometers, and most preferably between 0.01 and 0.2 micrometers. The uniform and fine particle size is less than the example 〇3 microns, in the super dielectric layer to provide superior dielectric strength in excess of volts per micron and low consumption factors, these properties provide increased reliability for high electrostatic capacity, high voltage ceramic materials. Provide a thin dielectric layer Capacities allow 5 to 10 times the electrostatic capacity of capacitors made of colloidal capacitors. This type of mlc, s is preferably an early-funded entity, such as titanium barium with metal oxide dopants, two types of interdigitated electrodes It burns in the body, and each extends to the other end of the body, and then two conductive terminals make self-contact with the two types at the other end. IML with X7R characteristics still has W s… S mouth temperature The coefficient is over the range of Q125C, and its change is 2% to 15%. In a preferred aspect of the present invention, when the ceramic material is X7R 胤 c, the size of the two T is: the grain size is less than 0.3 micron, and it contains 93 to 98% by weight Acid, Ma Wang's ceramics, and 2 to 7% by weight of other metals are oxidized .

II Tolerances for each barium 1 -28- This paper size is applicable to the Chinese National Standard (CNS) A4 (2) 〇χ 297mm 552250 A7 --- B7 Printed by the Employees ’Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs Preparation of the Invention (26) The following examples are not set to limit the field of the present invention. Example 1 Measure the effectiveness of dispersion of particles mainly composed of barium titanate in a non-aqueous solvent. Hydrothermally derived low-fire X7R After drying, the particles are dispersed in a solution of 80 toluene / 20 ethanol together with a phosphate dispersant. The hydrothermally-derived barium titanate wet cake prepared by X7R contains 72% by weight solids and 28% by weight water. Spin dry and empty the unit at 200 ° C. Twenty (20) pounds of dry x7R-modulated hydrothermally derived barium titanate particles and 6.7 pounds (3041.8 grams) of 80 toluene / 20 ethanol solvent The mixture was mixed to form a slurry. This slurry was mixed for 45 minutes with a DISPERSATORtm high shear mixer (Premier Mill), and 0.8 lbs (363.2 g) of RHODAFAC RS-410TM phosphate dispersant (Rh 〇ne_poulenc) 0 Measure the obtained slurry again Sample 丨) was dispersed in particle size, and the results are shown below and illustrated in Figure 1 A. · The slurry was ground horizontally in PREMIERtm for minutes (Premier Mill). The particle size of the obtained slurry (Sample 2) The distribution is re-measured, and the results are shown below and illustrated in Figure 1 B. The object was ground horizontally in PREMIERtm for 15 minutes (total 45 minutes). The particle size distribution of the obtained object (sample 3) was re-measured. And the results are as follows and illustrated in Fig. 1C. The solids at the end of the measurement were measured as ^:%.

Ticket holder I Grid Regulation Α4 S) Ｍ 公 (Please read the notes on the back first and write this page) i Binding. Line! 552250 A7 B7 Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs V. Description of the invention (27) 1. 45-minute high shear mixer 10.6 65.3 225.6 21.3 2. 30-minute horizontal grinding 0.136 0.205 0.347 2.6 3. 45-minute horizontal The method is to grind 0.133 0.192 0.356 2.7 yy again; tj phosphate dispersant can be dispersed in a solvent mixture of 80 toluene / 20 ethanol. This illustrates the ability of the X7R powder derived from the hydrothermal method to select a suitable dispersant in a non-aqueous solvent to produce a slurry with a particle (D90 / DlG) ratio of less than 3. It is believed that other solvents (such as those disclosed in the examples above), with appropriate dispersants, can be used to make a slurry containing particles (DWDm) in a ratio below 3. Although the results show that the barium titanate wet cake derived by the X7R modulation hydrothermal method can be dried and re-dispersed in a non-aqueous solvent to form a slurry containing particles (DWDM) with a ratio of less than 3 mash, the dried particles are Strongly coagulated particles that are not effectively coagulated when mixed with a male force. This kind of dry, solidified dispersion made of particles mainly composed of barium titanate has a submicron $ basic particle size, which requires substantially longer grinding to obtain particles of two meters? ®. Furthermore, it is believed that drying the cake ′ with heating, especially if the mash is carried out under the dish and / or for a long time, may affect the I coating film on the particles whose titanate 4 is king. Such potential negative effects include, truthfully, J t sub? The bonding of the hydrated oxide coating may become difficult to separate some coatings that do not peel off or break up the coatings whose particles are made of,, acid, or-. Example 2 Effective dispersion of non-aqueous II, mixture of barium titanate-based particles (please read the note on the back first to write this page) Order:. Lines 丨 · Smart scale 1 -30 297 (Mm) 552250 A7 B7 V. Description of the invention (28): The low-fire X7R particles derived from the hydrothermal method are subjected to a solvent exchange method, and then dispersed with a phosphate dispersant. The low-fire X7R particles derived from hydrothermal methods were initially in water. This water was replaced with a solvent mixture of 80 toluene / 20 ethanol. One kilogram (1 kg) of X7R-modulated hydrothermally-derived barium titanate was wetted, and contained 72% by weight of solids and 28% by weight of water, and slurried with one kilogram (1 kg) of ethanol. The slurry was placed in a Buchner funnel containing an ultrafiltration and mesh membrane, which was used as a filter tool. The ethanol was filtered through the formed wet cake, and the formed slit disappeared mechanically. Once the first filtration is almost complete, pour one kilogram (1 kg) of ethanol and filter through a calendar cake. Repeat this step as soon as the second pass is completed. After the ethanol had been filtered, one kilogram (1 kg) of toluene was added and filtered through a wet cake. This wet cake was left to dry to a solids load of 75% by weight. The resulting wet cake (859.3 grams) was mixed with a DISPERSATOR ™ high-shear mixture (Premier Mill) with 26.81 grams of RHODAFAC RS-410tm_ ester dispersant (Rhone-Poulenc). Let the high shear mixer mix the wet cake for 10 minutes (sample 4) and 30 minutes (sample 5). The particle size distribution of the obtained slurry was measured again, and the results are shown below and illustrated in Figs. 2A and 2B. IJ ---- 1 --------___ (Please read the note on the back to write this page first)-line. Printed samples of employees' cooperatives of the Intellectual Property Bureau of the Ministry of Economic Affairs Dio D50 D90 D90 / D10 4. 10 Min. High Shear Force Mixer 0.381 0.869 1.908 5.0 5. 30 min. High Shear Force Mixer 0.351 0.764 1.805 5.1 The results of the above experiments show that the solvent exchange method can be non-aqueous if necessary -31-This paper size is applicable to China Standard (CNS) A4 specification (210 X 297 mm) 552250 A7 B7 V. Description of the invention (29) The solvent replaces the water-soluble solvent, and then the appropriate dispersant is added to achieve an acceptable ratio (D9G / D1C)). The solvent exchange method provides the dispersion with more narrow particle size distribution, mixed with high shear force only (without horizontal grinding) for less time, and then obtained from a dry powder (as shown in Example 1, Sample Worker) Dispersion. And it is believed that in a non-aqueous solvent (by solvent exchange), the X7R powder derived by hydrothermal method and the selection of an appropriate dispersant can achieve less concomitant horizontal grinding (depending on other factors such as the size of the batch). machining. It is also believed that additional dispersants can be used to make the slurry containing particles with an acceptable (D90 / D1 ()) ratio. In addition to the foregoing, solvent exchange avoids the potential negative effects on the coating film of barium titanate-based particles from wet cake drying, especially during high temperatures and / or long periods of time. Example 3 Measure the effectiveness of using a silane coupling agent to promote the use of barium titanate-based particles in a non-aqueous solution. Hydrothermally derived powders were coated with methyltrimethoxylithium cloth. Methyldimethoxysilane provides a hydrophobic coating and is then applied to BaTi03 particles hydrothermally derived by x7R, as follows: 1. Mix 95 ml of ethanol with 5 ml of deionized water . The pH of the falling solution was adjusted to 4 using 0 μM HNO3. Methyltrimethoxysilane (5 g) was added to the acidified ethanol / water solution, and then stirred for 5 minutes to hydrolyze the three possible methoxy groups. 2. 舲 X7R withered BaT103, wet cake (70% by weight of solids) was diluted with liters of ethanol, and emulsified at 7,000 rpm for 1 minute. -------------- Install --- (Please read the note on the back first to write this page). Line! Printed by the Consumer Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs-32- 552250 A7 B7 V. Description of the invention (30) 3. Add the solution of ethanol / water containing hydrolyzed silane coupling agent to the particles of the X7R-modulated hydrothermal method. The slurry was then emulsified for 30 seconds at 7000 rpm. 4. Allow the resulting slurry to air dry for 24 hours to remove excess carrier. The obtained material was placed again in an air oven at 8 ° C for 12 hours until the powder was completely dried. The wet cake prepared by X7R was diluted with ethanol to obtain a very viscous suspension during the emulsification time. The obtained dried powder was on water The sink / float test was used to measure whether the hydrophobic coating film was successfully attached to the surface of the powder. The powder was gently ground in a mortar and pestleed, and then spread on the water surface in a beaker. The screwdriver blade particles floated on the surface of the water. But when some particles are agitated, they fall into the water. Therefore, when the X7R prepared wet cake was first diluted with ethanol, only part of the surface had a coating film. This part of the coating film was like a result of high viscosity, which caused the X7R wet cake was originally diluted with ethanol. High viscosity caused the coating to solidify and tended to disintegrate when mixed in the sink / float test.-Example 4 Measurement of the use of a silane coupling agent to promote the use of barium titanate-based particles in non-aqueous 'valley' For the effectiveness of dispersion in the agent, the hydrothermally derived X7R powder is coated with methyltrimethoxysilane as a coupling agent. The methyldimethoxy second pit provides a hydrophobic coating and is then applied to X7R On the BaTi〇3 particles derived from the hydrothermal method of the system, 95 ml of ethanol was mixed with 5 ml of deionized water as follows. The pH of the solution was adjusted to 4 with 0.1 M HNO. Trimethoxy stone yakaki (5 g) was added to the acidified ethanol / water solution, and then stirred for 5 minutes to let San-33- 丨 ii clothing --- (Please read the note on the back first to write this page). --- Printed by the Consumers' Cooperative of the Intellectual Property Bureau of the Ministry of Economic Affairs. The paper size is applicable to the Chinese National Standard (CNS) A4 specification (210 297 mm) 552 250 A7. 5. Description of the invention (31 possible methoxyl hydrolysis. 2. · X7R 碉BaTi〇3, wet cake (70 wt% solids ^) diluted with ethanol, and emulsified at 7000 revolutions per minute for 1 minute. • Ethanol with hydrolyzed mash coupling / Water solution was added to the slurry containing particles of X7R hydrothermal method, and then emulsified at 7000 revolutions per minute for 30 seconds. 4. Allow the slurry to air dry for 24 hours, to The excess carrier was removed. The resulting shellfish was placed in an air oven at 80 ° C for 2 hours, until the powder was completely dried. The dried powder obtained from water was subjected to a sinking / floating test on water to measure whether the coating film of water was successfully attached to the surface of the powder. The powder was gently ground in a mortar and pestleed, and then spread on the water surface in a beaker The particles float on the surface of two spoons and remain on the water surface even when agitated. Therefore, when the wet cake made by combining is first diluted with ethanol, it reaches a complete surface J. The wet cake prepared by slurry X7R is ethanol Dilute to get a good dispersion with low viscosity. When the hydrolyzed silane coupling agent solution is added, this is a good coating film. ~ Granules cooked by this artist will immediately thank all the parameters listed here as demonstration parameters. The method and equipment used in the present invention are intended for specific applications. Therefore, it should be noted that the foregoing specific examples are only examples and in the attached patents and scope and equivalent fields = can be implemented unless specifically stated. Λ -34- This paper scale thorn cap wealth (CNS) A4 size ⑵Qx 297 public love ^

Claims (1)

552250 A8 B8 C8 D8, Shen Qing patent scope L A slurry, dispersion or mud, which contains particles mainly composed of barium titanate, dispersed in a non-aqueous medium, the particles have a coating film, including metal oxides 2, metal hydrated oxides, metal hydroxides or organic salts of non-barium or titanium < metals, wherein when mixed using high shear forces, at least 90% of the particles have a particle size below 0.9 microns. 2. The slurry, dispersion or mud pack according to item 1 of the scope of the patent application, wherein the D9 / Dl () decile ratio of the particles having a particle size distribution is lower than 4. According to the slurry, dispersion or mud pack of item 1 of the patent application scope, the D9G / DlG decile ratio of the particles having a particle size distribution is lower than 3. 4. The slurry, dispersion or slurry according to item 1 of the scope of the patent application, wherein the D9 / d1 () decile ratio of the particles having a particle size distribution is lower than 2.5. 5. A slurry, dispersion or slurry according to item 1 of the scope of the patent application, wherein when the particles are dispersed by mixing with a high shear force, at least 90% of the particles have a particle size of less than 0.8 m. The slurry, dispersion or mud-slurry according to item 1 of the scope of the patent application, wherein when the particles are dispersed by mixing with high shear force, at least 90% of the particles have a particle size of less than 0.7 m. • A slurry, dispersion or mud beam according to item 1 of the patent application, where at least 90% of the particles have a particle size of less than 0.6 microns when the particles are dispersed by mixing with high shear forces. 8. A slurry, dispersion, or slurry according to item 1 of the patent application, wherein when the particles are dispersed by mixing with a high shear force, at least 90% of the particles have a particle size of less than 0.5 micron. 9. The slurry, dispersion, or mud according to item 1 of the scope of the patent application 'It (please read the precautions on the back ^! ^ Write this page) - 210X297 mm) Printed by A8 B8-^-C8, ___D8 ', Application for Special Purpose ^ ^ ^ ^ to a child, and the male force is mixed and dispersed, at least 90% of the particles have a particle size. Below 0.4 microns. ι〇 · Rooted in _ = Medium: ^ 凊 Patent No. 1 of the patent scope of the slurry, dispersion, or mud, when the Tian 忒 tzi is mixed and dispersed with Nannan shear force, at least 90% of the particles have a low particle size At 0.3 microns. 11 · Chonggen, Shi: A slurry, dispersion or mud of the first item of the patent scope, which 12 contains at least 50% by weight /. Of the particles. • A slurry, dispersion or slurry according to item 1 of the scope of patent application, which contains at least 60% by weight of the particles. The slurry, dispersion or slurry according to item 1 of the scope of patent application, which contains at least 75% by weight of the particles. The slurry, dispersion or mud according to item 1 of the patent application scope further contains a dispersant. 5. The slurry, dispersion or slurry according to item 1 of the patent application, wherein the particles include a coupling agent coated on the surface of the particles. 16. The slurry, dispersion or slurry according to item 15 of the scope of the patent application, wherein the coupling agent contains an organosilane. • A slurry, dispersion or mud according to item 1 of the patent application, which further contains an adhesive composition between 3 and 20% by weight, which includes a polymer that is dissolved or suspended and forms a film . 18. A slurry, dispersion or slurry according to item i of the patent application, wherein substantially all of the particles are homogeneous or spherical. 19. A slurry, dispersion or slurry according to item 1 of the scope of the patent application, wherein the particles are produced by a hydrothermal method. -36- This paper size is applicable to China National Standards (CNS) A4 (210X297mm) (Please read the notes on the back to write this page)-Installation · r line 552250 A8 B8 C8 D8 Intellectual Property Bureau staff of the Ministry of Economic Affairs Printed by Consumer Cooperatives 6. Scope of Patent Application 20. The slurry, dispersion or mud according to item [Scope of Patent Application], where the coating film covers most of the particle surface. 21. The slurry, dispersion, or slurry according to item 1 of the scope of the patent application, wherein the coating film contains at least one metal selected from the group consisting of 4bit, 4m, magnesium, bow, 4th, sharp, zirconium, giving, and information. , Mirror, group, tungsten, H, lead, nickel, zinc, boron, crushed, recorded, tin, dry, lanthanum, tungsten, or a combination of rare earth lanthanides. 22. The slurry, dispersion or slurry according to item 1 of the scope of patent application, wherein the non-aqueous medium contains an organic solvent. 23. A slurry, dispersion or slurry according to item 22 of the scope of application, wherein the non-aqueous medium contains a mixture of an organic solvent and water. 24. The slurry, dispersion or mud according to item 22 of the scope of the patent application, wherein the organic solvent is selected from the group consisting of benzene, methyl ethyl ketone, acetone, xylene, methanol, ethanol, propanol, 1,1,1-tri Ethyl chloride, tetrachloroethylene, amyl acetate, 2,2,4-triethylpentanediol-1,3-monoisobutyrate, -toluene, dichloromethane, rosin, ethanol, bromochloromethane , Butanol, acetone, methyl isobutyl ketone, cyclohexane, methanol, n-propanol, isopropanol, n-butanol, n-octanol, benzyl alcohol, glycerol, ethylene glycol, benzaldehyde, propane Acid, n-octanoic acid, ethyl acetate, butyric acid butyrate, n-hexane, and mixtures thereof. 25. The slurry, dispersion or slurry according to item 24 of the patent application, wherein the organic solvent is ethanol. 26. The slurry, dispersion or slurry according to item 1 of the scope of the patent application, wherein the non-aqueous medium contains a mixture of more than one organic solvent. -37- (Please read the precautions on the back to write this page first) -The size of the paper, -0 thread is applicable to the Chinese National Standard (CNS) A4 specification (210X297 mm) 552250 Employee Consumer Cooperatives, Intellectual Property Bureau, Ministry of Economic Affairs Printing A8 B8 C8 D8 VI. Patent application scope 27. The slurry, dispersion or mud according to item 26 of the patent application scope, where the mixture is selected from the group consisting of 72% trichloroethylene / 28% ethanol, 66% Methyl ethyl ketone / 34% ethanol, 70% methyl ethyl ketone / 30% ethanol, 59% methyl ethyl ketone / 41% ethanol, 50% methyl ethyl ketone / 50% ethanol, 80% toluene / 20% ethanol, 80% toluene / 20% ethanol, 70% toluene / 30% ethanol, 60% toluene / 40% ethanol, 70% isopropanol / 30% methyl ethyl ketone, 40% methyl ethyl ketone / 60% acetone, and mixtures thereof. 28. The slurry, dispersion or slurry according to item 27 of the scope of the patent application, wherein the non-aqueous medium is 80% toluene / 20% ethanol. 29. A method for forming a slurry, dispersion, or slurry, comprising: forming a slurry of particles mainly composed of barium titanate in an aqueous medium by a hydrothermal method; forming a coating film on the particles, and Including metal oxides, metal hydrated oxides, metal hydroxides, or metal organic acid salts other than barium or titanium; replacing non-aqueous media with aqueous media; and mixing far particles with high shear forces to disperse in non-aqueous media in. 30. The method according to item 29 of the patent application range, wherein the particles are mixed with a high shear force and dispersed in a non-aqueous medium until 90% of the particles have a particle size of less than 0.9 m. 31. A method according to item 29 of the scope of patent application, wherein the non-aqueous medium is used instead of the aqueous medium, including the solvent exchange method. 32. The method according to item 31 of the scope of patent application, wherein the solvent exchange method includes: passing a slurry of particles mainly composed of barium acid in an aqueous medium; and -38- This paper standard is applicable to the Chinese national ladder Standard (CNS) a4 size (210 X 297 mm) (Please read the notes on the back to write this page first)-Binding line 552250 ABCD VI. Patent application scope Intellectual property bureau of the Ministry of Economic Affairs employee consumer cooperative printed and filtered The particles are injected into a non-aqueous medium. 33. The method according to item 29 of the patent application, wherein the aqueous medium is used instead of the aqueous medium, including distillation. 34. The method according to item 33 of the patent application park, wherein the distillation method comprises: adding a non-aqueous medium to a slurry of particles mainly composed of barium titanate in the aqueous medium; and evaporating the aqueous medium. 35. The method according to item 29 of the scope of patent application, which further includes applying a coupling agent to the surface of the particles after replacing the aqueous medium with a non-aqueous medium. 36. The method according to item 29 of the scope of patent application, wherein This includes applying a coupling agent to the surface of the particles after forming a coating film on the particles and before replacing the aqueous medium with a non-aqueous medium. 37. The method according to claim 35 or 36, wherein the coupling agent contains organic seconds. · 38 · —A method for forming a slurry, dispersion or mud, comprising: mixing with a high shear force, dispersing a slurry mainly composed of barium titanate in a non-aqueous medium, until 90% of The particles have a particle size of less than 0.9 μm. The particles contain a coating film including metal oxides, metal hydrated oxides, metal hydroxides, or organic acid salts of metals other than barium or titanium. -39-(Please read the precautions on the back first to write this page)-Installation, 1T line This paper ruler is based on the standard of financial management (CNS) A4 (21GX297 mm)