TW201228989A - Heat insulation material and production method for same - Google Patents

Abstract

The purpose of the present invention is to provide a powder for which issues with conventional technology have been taken into consideration, that is capable of suppressing the occurrence of scattering or forming faults during forming or filling, and which displays sufficient heat insulation properties. Provided is a heat insulation material in a powder form, that includes silica and/or aluminum and a plurality of small particles with a particle diameter (Ds) of 5-30 nm and a BET specific surface area of 5-150 m2/g, and which has a heat transfer rate of 0.05 W/mK max., at 30 DEG C.

Description

201228989 VI. Description of the Invention: [Technical Field] The present invention relates to a heat-insulating material and a method of manufacturing the same. [Prior Art] / The average free path of air molecules at room temperature is about 100 run. Therefore, in a porous body having a void having a diameter of 1 〇〇 nm or less, the convection caused by the air or the heat transfer caused by conduction is suppressed, so that the porous body exhibits an excellent heat-dissipating action. According to the principle of the heat-dissipating action, it is known that the ultrafine particles have a low thermal conductivity and are suitable for a heat-insulating material. For example, 'Patent Document 艸 describes a heat-dissipating heat obtained by separately forming an ultrafine powder of cerium oxide into a porous body. The bulk density of the heat-insulating material is 0.2 to 1.5 g/cm 3 , and the specific surface area of BET (Brunauer_Emmett_Tellern) is 15 〜 400 m2 / g, the average particle size is 〇〇〇 1 ~ 〇 5, the cumulative total pore volume is 0.3 ~ 4 cm3 / g, the average pore size is! The cumulative micropore volume of the micropores below μηι is 7% by volume or more of the cumulative micropore volume in the molded body, and the cumulative micropore volume of the micropores having an average pore diameter of 0.1 μη or less is 10 of the cumulative micropore volume in the molded body. 〇/. the above. Patent Document 2 describes a method for producing a heat-insulating material which is formed by coating particles including a radiation absorbing scattering material or the like by a ring-shaped or spiral ultrafine particle having a ring inner diameter of 〇1 or less. The body-coated particles are mixed with the inorganic fibers or the porous body-coated fibers formed in the same manner as the porous coated particles to form a powder of the heat-insulating material precursor, and the precursor is subjected to pressure molding to produce a heat-insulating material. . Patent Document 3 discloses a fine porous body comprising fine particles having a primary particle diameter <RTIgt; [Patent Document 1] [Patent Document 1] Japanese Patent Laid-Open No. 2007-169158 (Patent Document 2) Japanese Patent No. 43676 No. 12 [Patent Document 3] 曰 Patent Patent Kaiping 1_1 〇3968 [Non-Patent Document] [Non-Patent Document 1] Independent Administrative Corporation New Energy and Industrial Technology Development Organization, 2005-2006 Results Report Energy-saving Technology Strategic Development Energy-saving Technology Practical Development "With Nano Porous [Drafting of the ultra-low-heat-conducting material of the composite structure] [Problems to be Solved by the Invention] The powder or the molded body described in Patent Documents 1 to 3 theoretically has a thermal conductivity close to that of still air. Rate, can be used as a thermal insulation material. However, the present inventors have found that when industrially using a heat-insulating material containing ultrafine particles as a main component as described in the patent documents 丨 3, there is a problem in the production steps. The question is specific to flb. The heat-insulating material having the ultra-secret particles as a main component is very fluffy and seems to be light and easy to handle. However, in the case of processing such as dusting and forming, small loose bulk density becomes an obstacle. When the powder having a small density is added, the first filament is filled into the forming mold, and the storage tank or the storage tank of the storage powder must be enlarged to The corresponding volume and the higher cost. In addition, == interrupts the agglomeration of the hot material in the step, and the looseness of the looseness of the storage material is changed according to the remaining amount of the heat-dissipating material in the storage tank. Therefore, there is a case where it is difficult to stably supply continuously. Such agglomeration of the formed raw material may cause insufficient filling in the mold, and the productivity is remarkably lowered. Further, in the case of the powder-shaped heat-insulating material, it is necessary to remove the air during the press-forming, but the pore volume of the porous body having the ultrafine particles as a main component as described in Patent Document 3 is relatively large. Since it is small, there is a tendency that degassing by decompression or the like takes a long time, and productivity is low. Further, when a bulky heat-breaking material having ultrafine particles as a main component is subjected to press forming, there is a tendency that a stroke increases. If the stroke is large, the powder in the vicinity of the pressurized portion is sufficiently compacted, but it tends to be insufficiently pressed away from the pressurized portion. For example, when the powder is filled in the molding die and pressurized from above, the upper portion of the powder which is filled in the molding die is sufficiently compacted, but the lower portion, that is, the bottom of the molding die, exists. The tendency of compaction becomes insufficient. If the compaction of the powder is uneven, lamination is likely to occur when the pressure is released. The layered layer refers to a phenomenon in which a molded article obtained by press molding is mainly peeled off into two or more layers in the thickness direction. If such layer peeling occurs, the product cannot be used as a product, and the yield is lowered, which is not preferable. In addition to the press forming, the heat-insulating material of the shape of the blade may be used by being filled in a material (for example, a bag or a tube of glass cloth), wound into a tubular shape, or the like. If the powder is easily scattered, the work efficiency when filling the material into the material is poor, so that in the case of such a use, the scattering of the powder becomes a problem and is expected to be solved. The present invention has been developed in the prior art as described above, and its object is to provide a method for suppressing the occurrence of scattering at the time of forming or filling, and exhibiting sufficient heat-dissipating properties. Powder. Further, an object of the present invention is to provide a molded body and a covering using the above powder, and a method for producing the powder. [Technical means for solving the problem] On the basis of the prior art, the inventors of the present invention have diligently studied to overcome the problem, and as a result, it has been thought that the average particle diameter of the cerium oxide powder or the alumina powder having a low thermal conductivity is appropriately set. Or, the BET specific surface area of the powder or the loose bulk density can be obtained by suppressing the occurrence of scattering or forming defects during molding or filling, and the present invention has been conceived. That is, the present invention provides a powdery heat-insulating material which is a powder containing a plurality of small particles including cerium oxide and/or aluminum oxide and having a particle diameter 〇3 of 5 nm or more and 3 Å or less. The BET specific surface area of the powder is 5 m2/g or more and 15 〇mVg or less, and 3 (the thermal conductivity under rc is 〇〇5 w/m·K or less. The bulk density of the above-mentioned heat-insulating material is preferably loose. It is 〇3〇g/cm3 or more and 0.35 g/cm3 or less. The above-mentioned heat-insulating material preferably further contains plural numbers including SiO 2 and/or oxidized ' 'particle size Μ 5 〇 nm or more ' 1 〇〇 _ or less The large particles, and the mass of the large particles is 60% by mass or more and 90% by mass or less based on the total mass of the small particles and the mass of the large particles. The above-mentioned material is preferably an infrared light-shielding particle. The thermal conductivity of the infrared light-shielding particles is preferably 0.5 μm or more and 30 μ'. Hot material 158675.doc 201228989 The total volume of the material is 0.02% by volume or more based on the total volume. % or less. ^ The thermal material is preferably one of 70 groups selected from the group consisting of a metal element, a soil metal, and a strontium, and contains a salt selected from the group consisting of an alkali metal element and an alkaline earth metal. In the case of at least one of the elements in the group, the content rate is 0.005 mass 00/〇 or more and 5% by mass or less based on the breakage of the 埶 何 何 何 何 何 何 , , , , In the case of a fault, the content rate is based on the total mass of the heat-dissipating material as the basis of the dry weight of 1 υ or more, and 1 () 〇〇 mass ppm or less. The upper _ free metal element, soil test metal element and strontium Preferably, at least one of the elements of the group is contained in the upper four large particles. The heat-insulating material preferably contains inorganic fibers, and the content of the inorganic fibers is preferably based on the total mass of the heat-dissipating material. The heat-insulating material is preferably contained in an amount of more than 20% by mass. The heat-insulating material preferably contains cerium, and the content of phosphorus is 0.002% by mass or more and 6% by mass or less based on the total mass of the heat-insulating material. Good for iron, iron content is broken The total mass of the thermal material is 0.005 mass% or more and 6% by mass or less. The present invention provides a heat insulating material obtained by molding the above-mentioned powdery heat insulating material. Preferably, the maximum load at a compression ratio of 〇 to 5% is 0.7 MPa or more. The heat-dissipating material obtained by the above molding is preferably a relative micropore volume ν of a micropore having a pore diameter of 〇〇5 pm or more and 0.5 μηι or less. The cumulative pore volume of the micropores having a pore diameter of 0.003 μηι or more and 15 μηηι or less is 1.58675.doc 201228989 The ratio R is 70% or more, and the pore diameter is 〇.〇5 μιη or more and 15〇(4) or less. The micropore volume V〇.〇5 is 0.5 mL/g or more and 2 mL/g or less. Further, the present invention provides the above-mentioned heat insulating material contained in the outer material. ‘The above outer cover material preferably contains inorganic fibers, or the outer cover material is a resin film. In addition, the present invention provides a method for producing a heat-insulating material, comprising the steps of: comprising a small particle comprising a silica dioxide and/or an oxidized oxide, and having an average particle diameter of not more than 2 nm and not more than 30 (10), and comprising two Oxide oxide and/or alumina, and the average particle size of 50 nm or more, 1 〇〇 μιη & large particles in the amount of large particles f relative to the ratio of the mass of the small particles to the mass of the large particles RL The mixture is mixed in an amount of 60% by mass or more and 9% by mass or less. Further, the present invention provides a method for producing a heat-insulating material, comprising the steps of: arranging cerium oxide and or aluminum oxide, and having an average particle diameter of 5 (10) or more and 30 Å or less, and And comprising at least one element selected from the group consisting of a metal element of the metal element and the soil element, and an average particle diameter of 5 〇 nm or more and 1 (10) pm or less: The inorganic mixture is obtained by mixing the mass of the large particles with respect to the total mass of the small particles and the mass of the large particles of 6% by mass or more and % by mass or less. Further, the present invention provides a method for producing a heat-insulating material as described above, comprising: a housing step of accommodating the following inorganic mixture in a molding die, the inorganic mixture being massed with respect to small particles The ratio of the mass to the total mass of the large particles is 6% by mass or more and the column mass% or less is 158,675.doc

S 201228989, and containing small particles comprising cerium oxide and/or aluminum oxide and having an average particle diameter of 5 nm or more and 30 nm or less, containing cerium oxide and/or aluminum oxide, and being selected from alkali metal elements At least one element selected from the group consisting of an alkaline earth metal element and cerium, and a large particle having an average particle diameter of 5 〇 nm or more and ι 〇〇 μπ or less; and a forming step of forming the inorganic mixture; and the forming step is The steps are as follows: (a) the surface is pressed to the inorganic mixture by a molding die, and heated to 40 (TC or more); or (b) the inorganic mixture is formed by pressurization, and then the temperature is 400 ° C or higher. In the forming step, it is preferable to set the molding pressure so that the bulk density of the heat-insulating material is 0.25 g/cm 3 or more and 2.0 g/cm 3 or less. The method for producing a heat-breaking material, comprising: a housing step of accommodating the following inorganic mixture in a forming mold, the inorganic mixture being massed with respect to the mass of the small particles and the mass of the large particles The total proportion of the core is 60 mass% / 〇 or more, and 90% by mass or less, and contains small particles including cerium oxide and/or aluminum oxide and having an average particle diameter of 5 nm or more and 30 nm or less. Cerium oxide and/or oxidation, and at least one element selected from the group consisting of an alkali metal element, an alkaline earth metal element and cerium, and having a large particle diameter of 5 〇 nm or more and 1 〇〇 μηη or less a forming step of forming the inorganic mixture; and a cutting step of cutting a portion of the formed body obtained by the above forming step; and the forming step is the step of: surface so that the bulk of the formed heat-insulating material is 0.25 g/cm3 or more and 2.0 g/cm3 or less, 3) pressurizing the inorganic mixture by the molding die, heating step 158675.doc 201228989, or (4) dusting by using the above-mentioned forming die The inorganic mixture is formed by a heat treatment at a temperature of 9400 C or higher. [Effects of the Invention] According to the present invention, it is possible to provide scatterability at the time of molding or filling. A heat-insulating material which is excellent in the formation of defects during molding, and which has good moldability, and a manufacturer thereof. Further, the present invention can also provide a method for forming (4) a heat-dissipating material. The heat-resistant material and the heat-dissipating material covering body which accommodates the material other than the heat-insulating material. [Embodiment] Hereinafter, the form for carrying out the invention (hereinafter referred to as "this embodiment J") will be described in detail. The present invention is not limited to the following embodiments, and various modifications can be made within the scope of the gist of the invention. [1] Powder-like heat-insulating material [1 -1 ] Oxide oxide, alumina This embodiment The heat-breaking material contains a plurality of small particles of dioxo prior and/or oxidized' as a powder. If the content of the silica dioxide and/or the ::chain in the heat-insulating material is 50% by mass or more, it is preferable because the solid conduction causes a small one. When the rate of the oxidized particles and/or the oxidized particles is 75 mass% or more of the powder, the adhesion between the powders is increased, and the scattering of the powder is reduced, which is more preferable. In addition, in the present specification, the cerium oxide particles are not limited by the components represented by the formulas §1〇2, but also the materials containing Si〇» Λ ν 2 A particle containing a gold compound in addition to Si〇2 is contained. The dioxoparticle may contain Si and a salt with various other elements or a complex oxygen 158675.doc 201228989, and may also contain a hydrated oxide such as a hydroxide, or may have a sulphuric acid base. . In the present specification, the oxide-containing particles are not only composed of particles composed of components represented by the composition formula Al2〇3, but also include a material containing Al2〇3, and contain metal components in addition to Al2〇3. Particles of other inorganic compounds. In addition to pure oxidation, the oxidized particles may contain AUx and salts or composite oxides with various other elements, and may also contain hydrated oxides such as hydroxides. The oxidized chain in the dioxo prior particles and/or the oxidized particles may be crystalline, may be amorphous, or may be a mixture of the same, but if amorphous, the solid conductive material in the heat-insulating material The heat transfer is small and the heat-dissipating performance is high, so it is preferable. Specific examples of the cerium oxide particles are as follows. It is called "cerium oxide", "the oxide of quartz J. It is a partial oxide of cerium. Composite oxide of cerium oxide-alumina or cerium."

Na, Ca, K, Mg, Ba, +, and any of the sulphuric acid salts (glass). A mixture of oxides, partial oxides, salts or composite oxides, oxidized or oxidized, etc., with an oxide, a partial oxide, a salt or a composite oxide.

An oxide of SiC or SiN. Specific examples of the alumina particles include the following. An aluminum oxide called "alumina". It is called oxidation of α_oxidation 1 ul, γ-oxidation, and β-oxidation. Part of the oxide. 158675.doc -]]- 201228989 and other composite oxides. Aluminate of any of Ce, B, Fe and Si, oxidized stone, oxidized or zeolite

Na, Ca, K, Mg, Ba, salt (glass). A mixture of oxides, partial oxides, salts or composite oxides (--cerium oxide or titanium oxide, etc.) of the elements other than those of the oxides, or oxides of partial oxides or complex oxides. An oxide of aluminum carbide or aluminum nitride. Preferably, the cerium oxide particles and/or the oxidized mineral particles are used at the temperature at which the heat-insulating material is used. Specifically, it is preferred that the weight of the silica wire and/or the oxidized grain is not reduced by more than 10% when the temperature is maintained at the highest use temperature of the heat-insulating material for one hour. Further, from the viewpoint of maintaining the viewpoint of the heat-dissipating property or the shape retention during molding, the dioxo prior particles and/or the oxidized particles preferably have water resistance. Specifically, it is preferably relative to :25. . The water is 1 〇〇 g, and the cerium oxide particles and/or the alumina particles are dissolved at less than 0.1 g Å, preferably less than 001 g. The specific gravity of the cerium oxide particles and the alumina particles is preferably 2 Å or more and 5 Å or less. When it is 2.0 or more and 4.5 or less, the bulk density of the heat-insulating material is smaller, and therefore it is more preferably 2 Å or more and 42 or less. Here, the specific gravity of the cerium oxide particles and the oxidized particles refers to the true specific gravity determined by the pycnometer method. As described above, it is known that a porous body having a void having a diameter of 100 nm or less has a low thermal conductivity and is suitable for a heat-insulating material. In the case of obtaining such a heat-insulating material, the method of forming fine particles having a particle diameter of 1 〇〇 nmU by pressing or the like is relatively simple. However, when a porous body is produced by, for example, adding a powder of a so-called super 158675.doc 12 201228989 microparticle having a particle diameter of about 20 nm, the volume of the powder is not likely to be produced. The shock is easy to become large, and the stroke during pressurization increases. As a result, the production time (four) time), that is, the powder is filled into the forming mold, and the dust is removed, and the pressure is removed. The powder is pressed out from the forming mold to pressurize the powder. The time taken for molding the obtained molded body becomes long, and delamination tends to occur, and the + yield is high, so that productivity tends to be lowered. Further, since the bulk density is small, there is a tendency that it is difficult to uniformly fill the molding die. Further, for example, in the supply step of the powder, it is easy to scatter when injecting the storage tank hopper or to be easily aggregated in the storage tank hopper, and molding defects are likely to occur at the time of press molding. If the amount of the ultrafine particles is reduced to suppress the molding defects, and the amount of the inorganic fibers is increased, the heat-dissipating property is lowered to the extent that the use as a heat-insulating material is hindered. "Inventors have found that by adjusting the bet specific surface area of the powder-shaped heat-insulating material to an appropriate range, the manufacturing apparatus such as a press forming apparatus can be miniaturized" and the heat-insulating material exhibits excellent breakage. Thermal performance. Further, when the bet specific surface area is adjusted to an appropriate range, it is surprisingly found that even a particle (large particle) having a particle size which is not so small as a raw material of a heat-insulating material, which is not suitable as a material for the heat-insulating material, is used as a raw material by It is also possible to obtain a heat-insulating material which can coexist with both the BET specific surface area and the excellent heat-dissipating property by mixing with ultrafine particles (small particles) in an appropriate amount. As a result of research by the present inventors, it has been found that particles containing cerium oxide and/or aluminum oxide and having an average particle diameter of 5 nm or more and 3 Å or less are contained as small particles, and include cerium oxide and/or aluminum oxide, and A particle having an average particle diameter of 5 〇 nm or more and 100 or less is used as a large particle, and the ratio of the mass of the large particle 1:58675.doc 13 201228989 to the total mass of the small particle and the mass of the large particle is 60 parts by mass or more and 9 9% by mass or less are mixed, and it is easy to adjust the BET specific surface area of the heat-insulating material to 5 plus 2 or more and 15 〇 m 2 /g or less to obtain the volume of the powder before pressurization. It is not too large, and it is easy to fill into a forming mold, and it is not easy to fly or agglomerate powder. When mixing small particles and large particles to prepare a powder, it is preferable to combine small particles with large particles. The collection is mixed, and the "average particle size" is in each set. On the other hand, in the state of a powder containing small particles and large particles, whether it is a continuous particle distribution or a particle size distribution having a plurality of maximum values, there is no influence on heat conduction, as long as it is described later. It is enough to satisfy "containing a small number of small particles". In addition, although the particle size distribution affects the BET specific surface area, it is not a direct and necessary condition to have a plurality of maximum values. Therefore, the present inventors have recognized that it is necessary to be a necessary condition for a heat-insulating material ("containing a plurality of small particles", and it is not necessary to specify the characteristics of small particles and/or large particles contained in the powder." The inventors have further studied the loose bulk density of a powdery heat-dissipating material mixed with small particles and large particles, if the above & 〇~ is less than 60% by mass In the range of the case, there is a tendency that the bulk density is small regardless of how it is loosely filled. On the other hand, if the core is 6 〇 mass% or more, the bulk density of the powdery heat-insulating material tends to increase. (See Fig. 1). In other words, if the content is 60% by mass or more, the loose bulk density of the powdery heat-insulating material becomes an appropriate size, and the volume before pressurization is 158,675.doc 201228989 ΓΓ, which is easy to fill to In the forming mold, the reason is not clear. It is considered that the filling state of the small particles and the large particles is different depending on the RL, and if it is less than 60% by mass, the gap formed by the small particles and the large particles is relatively large. Therefore On the other hand, when the volume of the powdered heat-insulating material is less than or equal to (4)% or more, the filling state of the small particles and the large particles becomes denser, and the voids are reduced, and the powder is in a state of powder. On the other hand, it is presumed that the thermal conductivity which is not excellent even though the void is reduced is that it is mixed in a range of 60% by mass or more and 9% by mass or less. In the case of small particles and large particles, the filling state becomes relatively dense, but the voids formed by the particles form a bottleneck of heat transfer between the stations. It is easy to suppress spatial heat conduction. In addition, the particles of different particle sizes are mixed and will be bribed. The specific surface area is adjusted to the range of the material, the adhesion or the physical friction angle between the particles, that is, the interparticle friction (four), the friction angle between the layers inside the powder, that is, the internal friction angle, the chargeability, etc. change or permit the relaxation only by the ultrafine particles. The heat-dissipating material is easily scattered and easily aggregated. That is, the heat-insulating material preferably contains two or more kinds of dioxobic particles and/or oxidized particles, especially In the case where two kinds of particles having different particle diameters, that is, small particles and large particles containing cerium oxide and/or oxidized oxide are contained, the mass of the particles is preferably the mass of the small particles and the mass of the large particles. The ratio is 60% by mass or more, and 9% by mass. If the content is less than 60% by mass, the powder tends to be easily scattered. The right is more than 90% by mass, and the heat-dissipating property is liable to decrease. The tendency of pressure molding is difficult. From the viewpoint of heat-dissipation performance, the ratio of the mass of the large particles of 158675.doc -15· 201228989 is preferably 60 mass%, more than 〇, 85% by mass or less, and even more preferably 65. 5% by mass or more, and more preferably 65% by mass or more, and more preferably 5% by mass or less. As described in Non-Patent Document 1, a precursor of a heat-insulating material having ultrafine particles as a main component exists in pressurization. When the pressure is released after the molding, the molded body tends to expand greatly. This expansion is called spring back. In the case of a molded body obtained by press molding ultrafine particles containing ultrafine powder as a main component, the molded body obtained by the ultrafine particles as a main component of the present invention has a problem that rebound occurs and a molding defect occurs in some cases. The fine porous structure does contribute to the reduction of heat conduction of the heat-insulating material, but if the air is not sufficiently removed during press forming, rebound is likely to occur. When the large particles are blended, the rebound tends to be suppressed at the time of molding as compared with the case of the small particles. When the blending amount is 25% by mass or more, the effect of the suppression is remarkable. As described above, if the amount of the large particles is too large, the heat-dissipating property tends to decrease. Therefore, the ratio of the large particles to the small particles of the heat-insulating material is preferably such that the BET specific surface area and the powder-like heat-dissipating material are scattered. The manner in which the springback of the formed, heat-insulating material is suppressed and the thermal conductivity reaches a desired value is determined by considering the balance. The heat-insulating material described in Patent Document 2, as disclosed in the non-patent document, has a crack-like forming defect on the surface perpendicular to the pressing surface during press forming. If such a forming defect exists in the heat-insulating material, not only the heat-breaking material is damaged, but also the heat-dissipating property is lowered, so that it cannot be used as a product, and the yield is lowered, which is not preferable. Further, the heat-insulating material having ultrafine particles as a main component tends to be delaminated after press molding. The layer referred to as I58675.doc 201228989 refers to a phenomenon in which the molded article obtained by press molding is mainly peeled off into two or more layers in the thickness direction. If such a layer peeling occurs, it is not good to make a decrease in the yield of the product. It is a large particle and a small particle having cerium oxide as a main component, and the particle diameter of the large particle is 4 〇 nm to i 〇 _, and when the particle diameter of the small particle is 5 nm to 3 G nm, if large particles are present In the powder, the ratio is a ratio that is preferable for suppressing the rebound, and it is also difficult. There is a tendency to create stratification. As described above, if the blending amount of the large particles is 60% by mass or more, the BET ratio is loose, and the loose bulk density is reduced to a moderately large J stroke, and if the average particle diameter of the large particles and the small particles is within the above range Then, the filling state of the particles becomes a better state, and there is a tendency that the layering suppression effect becomes remarkable. In the present specification, the term "loose filling bulk density" means a value obtained in accordance with the measurement order of "initial bulk density" of m r 1628. Specifically, the measurement is performed according to (1) to (4) in the order of the "7" measurement method, that is, (.1) the mass of the container is measured by using a balance measurement; (7) the sample is loaded into the measurement container through the sieve. Until it overflows; at this time, it is not possible to apply vibration to the measuring container or to compress the sample; (3) Scrape the powder raised from the upper end surface of the measuring container with a squeegee, and this _ ' is to make the squeegee self-scraping The direction is inclined to the rear and used to the plate so as not to compress the powder; (4) The quality of the sample is calculated by measuring the mass of the measuring container together with the mass of the measuring container by the balance measurement. The difference between the initial bulk density and the officially measured bulk density of JIS R 1628 is 1:58675.doc •17· 201228989 0.3 °/. On the other hand, in the case of the powdery heat-insulating material of the present embodiment, there is a case where the difference between the initial bulk density and the original bulk density is largely different. However, the present inventors have found that the ease of delamination and the "initial bulk density" at the time of press forming a powdery heat-insulating material are important indexes, and the present invention has been completed. One example of a measuring device for loose bulk density is shown in Fig. 2. The distance between the front end of the funnel installed at the lower part of the screen and the measuring container is set to 2 〇 3 〇 mm °. The loose packing density of the powder-like heat-insulating material is preferably 0 030 g/cm 3 or more and 0.35 g. /cm3 or less. If the bulk density of the loose packing is less than 3 〇g/cm, the volume of the heat-insulating material is large, for example, there is a tendency for the apparatus required for press forming to be enlarged, and there is a tendency to become easily scattered and agglomerate. It is not good. The loose bulk density of the powdery heat-breaking material can be controlled by adjusting the ratio of the mass of the large particles to the total mass of the small particles and the mass of the large particles. The BET specific surface area is 5 m2 / g or more, 丨 5 〇 m 2 / g or less, and the thermal conductivity at 30 t is 0.05 w / m · "lower" and the loose bulk density is 0.030 g / cm 3 or more, 〇 In the case of 35 g/cm3 or less, large particles having a relatively large average particle diameter (for example, 5 〇 nm to 1 〇 μιη) are selected, or the ratio of the mass of the large particles is set to be small (for example, 6 〇 mass% or more) 5% or less of ribs) is easy to adjust. At this time, in many cases, the conductivity of the powder is less than G.G35W/mK, that is, the loose filling is adjusted by making the operation easy. The bulk density will adjust the thermal conductivity to a better range for the thermal material. '", if the loose fill density exceeds 〇.35 g/cm3, there is thermal insulation performance. 18·158675.doc

201228989 The tendency of lowering is not so good, so that the volume before pressurization is suitable for filling into the forming mold, ',', 〇1 / 3 is more preferably 0.03.5 g/cm3 or more and 0.3 g /cm or less, in the case of heat-dissipating performance, when it is 0.040 g/cm3 or more and 〇25 g/cm3 or less, and more preferably contains infrared light-shielding particles, the tendency of the heat-dissipating material is stronger, so that it is added. „The volume == is easy to fill the forming mold and the high temperature region; the thermal insulation performance is good, the loose bulk density is preferably 0.045 g/cm3 or more and UgW or less, more preferably 〇.〇5g/ More details of cm3 and above, 〇25~ to ★ more preferably G.G5 g/em or more, 〇2Q g/em3 with p-infrared shading particles will be described later. About small particles and large particles, Jin, you丨& π # can be calculated by, for example, self-heating materials: particles, large particles, and measuring the mass of each. The method of separating small particles and large particles is not particularly limited, and the revised version 6 (Maruzen) The eighth grade of the record is used for the work of the J6 war knife level or grading As a well-known classification method, wet classification or dry classification can be cited. As a machine for performing wet classification, a gravity classifier (deposition knife class machine), a cone classifier, and a hydraulic classification can be cited. Machine, siphon classifier, centrifugal classifier, liquid cyclone, sputum classifier, grip classifier, Aklns type, spiral classifier, cupping classifier, hydraulic separator, decanter I As a machine for performing dry classification, a sieve such as a vibrating screen, a surface sieve, a rotary sieve, a double cylinder sieve, a gravity classifier, a knife-level machine, a wind classifier, and a free scroll type centrifugal classification may be mentioned. Machine, cyclone, scattering type classifier (dlSpersi〇n separat〇r), forced scroll type centrifugation 158675.doc 201228989 classifier, vortex classifier, Micr〇plex classifier, micro Separator, Accucut, Overspeed Separator, Sturtevant Classifier, Turbopiex, Cyclone Air Separator, 离心·SEPA Centrifugal Classifier, Shutter Type Classifier, ^τ〇η_η Classifier, E An inertia classifier such as an ibow Jet classifier or a modified virtual impactor, etc. The classifier may be selected according to the particle size of the small particles to be separated and the large particles, and the classifier may be used in combination. The particle size of the oxidized peak can be scanned by field emission

Field Emission Scanning Electron MiCroscopy) was measured by observation. In the case of small particles, the magnification (for example, _〇 times) is set so that particles of 5 (10) or more and 30 (10) or less can be observed, and a "representative field of view" is randomly selected from the heat-dissipating material for observation. The so-called "representative vision" is not a special field of view, but is expressed in any heat-dissipating material that is selected, and the field of vision is shared to a certain extent. In the case where the heat-dissipating material is a heat-insulating material containing particles larger than the size of the small particles, it is also possible that most of the field is observed, but the field of view observed only in the minimum-part is not a representative field of view. 'So not choose this field of view. In the case of Yu Zhizhi 1 observation, the loss between the materials is less than the first. . Observe the left and right, select the ordinary: see the wild, and then observe at a magnification of 1〇_倍. Seeing the representative field of view, small particles above σ, you can observe two "breaking hot materials" in this field of view can be judged as "contained but 疋, even if the initial observation of D No more than 2 small particles were observed in the field of view. I58675.doc •20- 201228989

In the case of f, as long as 100 representative fields of view are observed, 100 small particles can be observed in the A juice, that is, ", σ ± ΒΒ rh ^ 3 has a small pull". That is, as long as two or more small particles can be observed in the representative cross-sectional field of view initially observed, it means "containing small particles", if (7) is not observed in the representative cross-sectional field of view observed initially. In the case of two or more small particles, as long as 100 small particles are observed in a total of 100 representative cross-sectional fields, "small particles are satisfied". Particles are not necessarily circular particles, but may also be elliptical. The diameter of the particles is determined by the diameter of a circle of equal area. The diameter of a circle of equal area is the diameter of a circle having the same area as the projected area of the particle, also known as the Heywood diameter. Even if an elliptical particle is present, if the area is, for example, 78 - an area corresponding to a circle having a particle diameter = 1 〇 nm, the particle diameter can be regarded as H) nm. In the case where the heating step is included in the manufacturing step, it is also possible that there is a possibility that the small particles are mutually melted and then the boundary cannot be recognized, but as long as the cross-sectional area of the melt followed by the elliptical shape is spectroscopy - η 2 (corresponding to the particle diameter) =3 〇nm circle area) below, that is, a "small particle". In the case where the melting is caused by the degree of enthalpy, the boundary can be recognized at the magnification, and the particle diameter of each particle (equivalent to the diameter of the equal area circle) can be measured. Regarding whether or not the small particles are included, the particle diameter of each particle can be determined by the diameter of a substantially equal-area circle, so that it is not necessary to obtain the average value of the particle diameters, and it is determined that the heat-dissipating material is grasped based on the entire collection of small particles. When the average value of the particle diameter is obtained for the purpose of the physical property, etc., the magnification is set so that particles of 1:58675.doc • 21 · 201228989 nm or more and 3 〇 nm or less can be observed, and (10) or more particles are observed. 'It is sufficient to calculate the diameter of a substantially equal area circle and calculate it by number average. The small particles contained in the heat-insulating material can be adhered to a conductive tape such as a carbon adhesive tape adhered to the sample stage by observation under the following condition 'device, and coated at about 2 nm to s. Sample for microscopy. The Os coating can be carried out using, for example, a Hunger Coating Machine (Hpc_lsw type, manufactured by Device Co., Ltd.). A scanning electron microscope (su_70, manufactured by Hitachi High-Techn Co., Ltd.) was used as a microscopic inspection apparatus, and measurement was performed under the conditions of an acceleration voltage of 1 〇 kv. The particle size 〇5 of the small particles is 5 nm or more and 30 nm or less. If the enthalpy is 5 nm or more, the chemical stability of the small particles tends to be stabilised compared with the case where Ds is outside the above numerical range, and the heat-dissipating property tends to be stable. If 〇5 is 30 nm or less, compared with the case where Ds is outside the above numerical range, there is a small contact area between small particles, and the heat transfer caused by solid conduction of the powder is less. Small tendency. When Ds is 5 (10) or more and 25 nm or less, it is preferable from the viewpoint of thermal conductivity, more preferably $ nm or more, 20 nm or less, and even more preferably 5 nm or more '18 _ or less' is particularly preferably 7 nm. Above, below 14 nm. The particle size DL of the large particles satisfies ds < Dl. The DL is preferably 5 〇 nm or more and 1 〇〇 μ ΐΏ or less. Dl can be obtained by the same method as described above. If it is 50 nm or more, there is a tendency that the rebound in the molded body is small when the powdery heat insulating material is molded. If it is 1 〇〇 μηη or less, there is a tendency that the thermal conductivity is small. The particle size of large particles!^ can also be 8〇 nm or more, ι〇〇 158675.doc

In the case of 50 nm or more and 50 μm or less, when the heat insulating material contains inorganic fibers or infrared light-shielding particles, it is preferable to be evenly present in such a manner. When the DL is 50 nm or more and 1 μm or less, the adhesion of the particles is large. The particles are less likely to fall off from the powder, and more preferably 50 nm or more and 5 μη or less. When DL is twice or more as Ds, it is preferable to reduce the rebound when the powdery heat-insulating material is formed. If the ratio of the small particles to the large particles is larger than 3 times, the volume of the mixed powder of the small particles and the large particles is large, and the volume of the powder is small, the workability is high, so that if the volume is more than 4 times that of 1^, then The particle size difference between the small particles and the ^ particles is large, and when the small particles are mixed with the large particles, the large particles are easily dispersed with respect to the small particles, which is more preferable. From the viewpoint of solid heat transfer by particle agglomeration (4), it is preferred that the respective particles are dispersed. That is, it is preferable that there is no portion where the large particles are in direct contact with each other and joined. The gap between large particles due to the fact that large particles are not directly bonded is filled by small particles, and the particles are not easily in direct contact with each other. Therefore, there is no heat transfer path in which the solid conduction is large in the heat-insulating material, and the thermal conductivity of the entire heat-dissipating material is easily lowered. Further, by filling the gaps between the large particles by the small particles, the voids present in the heat-dissipating material are reduced, and the convection or heat transfer caused by the air is suppressed: the thermal conductivity of the heat-dissipating material as a whole is easy. reduce. (2) It is preferable that the heat-insulating material contains a water repellent agent from the viewpoint of deterioration in workability, deformation of the molding, production of crepe, and the like when the water is infiltrated into the powder or the formed crucible. Examples of the water repellent include an ant-based water repellent such as a stone, a poly-ethylene phthalic acid-ethyl phthalate copolymer, a polysulfide resin, and a kiln of a kiln, a kiln, and an oxy group. Water repellent; full appearance: (4) i 58675.doc •23- 201228989 Salt, perfluoroalkyl phosphate, perfluoroalkyltrimethylammonium salt and other oxime water repellent; containing alkyl or perfluoro group a decane coupling agent such as alkoxy decane; a tridecyl gas decane or a decylating agent such as 1,1,1,3,3,3-hexamethyldiazepine. These may be used in one type or in two or more types. These may be used as they are or in the form of a solution or emulsion. Among them, a wax-based water repellent or a hydrazine water repellent is preferably used. As for the content of the water repellent in the powder, the quality of the whole powder/the quality of the water repellent is preferably UK^OMOO/O, more preferably 100/ 2〇~1〇〇/〇5, and more preferably 100/10~100/1. The method of adding the water repellent is not particularly limited, and for example, a method of adding the water repellent to a solvent obtained by diluting the water repellent with water or an alcohol such as '-(four) powder mixture' and then drying the powder; A slurry is prepared in a solvent such as water or alcohol, a water repellent agent is added thereto, and the method is applied and filtered, followed by drying; or steam treatment using gas methacrylate or the like. When the heat-resistant material has a specific surface area of A5g/m2 or less and 15 Gg/m2 or less, the amount of the water repellent agent required to impart a water repellency effect is small. Further, if the amount of the water repellent used is less #, there is also an advantage that the amount of escape gas (Qutgas) released when the heat-insulating material is exposed to a high temperature is small, and the influence of the environment is small. T1·2] Inorganic fiber When the heat-insulating material is formed, the heat-insulating material preferably contains inorganic fibers. The mechanical fiber heat-dissipating material has the advantages of less particle enthalpy of the material, and higher productivity when formed by press molding. Further, the heat-insulating material containing the machine fiber has an advantage that it is not easily collapsed and is easy to handle. In the state of the blade body, there is less scattering, so it is better in terms of operation. I58675.d〇c

S •24· 201228989 The term “reduced fiber” refers to a ratio of the average length of inorganic fibers to the average thickness (aspect ratio) of 10 or more. The aspect ratio is preferably ι〇=up; the shape of the heat-dissipating material can be formed with a small pressure, and the productivity of the juice-heating material is 'better'; From the viewpoint of the bending strength, it is more preferable that the aspect ratio of the fiber can be determined from the average value of the thickness and length of the inorganic fiber by FE_SEM. The inorganic fibers are preferably monodispersed and mixed in the powder, but may be mixed in a state in which the inorganic fibers are entangled with each other or in a state in which a plurality of inorganic fibers are bundled in the same direction. Further, in the monodispersed state, the orientation of the inorganic fibers may be uniform in the same direction, but from the viewpoint of reducing the thermal conductivity, the inorganic fibers are preferably aligned in a direction perpendicular to the heat transfer direction. The method of aligning the inorganic fibers perpendicularly to the heat transfer direction is not particularly limited. For example, when the outer material or the construction site is filled with the powder-shaped heat-insulating material, the powder is made of a hot material: The filling is dropped to the filling portion, and the inorganic fiber has a tendency to align perpendicularly to the heat transfer direction. In the case of a heat-formed material which is formed by pressurization, for example, by pressurizing in the same direction as the heat transfer direction, it is easy to align the inorganic fibers originally aligned in the heat transfer direction in a direction perpendicular to the heat transfer direction. . The example of the right non-inorganic fiber can be exemplified by continuous glass fiber (filament), 2 Al2〇3 B2〇3-Ca〇, glass fiber, glass thief (8)〇”Αΐ2〇3·

La〇'Na2〇), test glass fiber (SKVzr〇2-Ca〇_Na2〇), rock 蜮 (basalt mineral wool) (SicvAl2(VFe2〇3_Mg0_Ca〇), slag (si〇2_ 3 Mg〇CaO) , pottery-bright fiber (mullite fiber) (Ai2〇3_Si〇2), I58675.doc -25· 201228989 cerium oxide fiber (Si〇2), alumina fiber (A12〇3_si〇2)' potassium titanate Fiber, alumina whisker, tantalum carbide whisker, tantalum nitride whisker, calcium carbonate whisker, basic magnesium sulfate whisker, calcium sulfate whisker (gypsum fiber), zinc oxide whisker, yttria fiber, carbon fiber , graphite whisker, phosphate fiber, AES (Alkahne Earth Silicate) fiber (Si〇2_

CaO-MgO), natural minerals such as limestone, sepiolite, erbium, and hydrotalcite. Among the inorganic fibers, it is particularly preferable to use AES fiber which is biosoluble in human body safety (Alkaline Earth is priced at (10). As the fiber, for example, an inorganic glass of Si〇2-Ca0-Mg0 type (inorganic polymer) The average thickness of the inorganic fibers is more than μηι from the viewpoint of preventing scattering. In the case of a heat-insulating material, the preferred (four) inorganic fibers are suppressed from the viewpoint of heat transfer caused by solid conduction. The thousand-thickness can be obtained by using F to cut the thickness of the inorganic fiber and to average it. 対 In view of the powder detachment of the heat-dissipating material in the shape of the heat-dissipating material, The powder mass is preferably more than 0% by mass, and the thermal conductivity is preferably G.05 W/m. κι; from the viewpoint of G.05 W/m. κι; In the case of particles, from the viewpoint of the ease of mixing with the red sun shading particles, 'inorganic good is 0.5% by mass: 1:11_10@旦0/3 ^ ^ Buy! Above, 18% by mass or less 'is small In terms of point of view, further p has a brother, a dense moon and thus a better 0.5 More than % by mass, 〇 158675.doc

S -26· 201228989. The content of the inorganic fibers can be determined, for example, by self-centering. 'Mixing inorganic fiber D·3】Infrared light-shielding particles Infrared light-shielding particles are required for heat-breaking properties at high temperatures. The term "infrared material" is preferably a material which reflects, scatters or absorbs light. By mixing infrared light-shielding particles in the infrared, it is possible to suppress the heat of the material, so that in particular, 20()t, the radiation is caused by the radiation.疋2〇〇 “The heat-dissipating performance of the upper to the temperature zone is better than that of the 1st chemistry: for example, oxidation error, (four) error, stone formation: titanium oxide, iron oxide, copper oxide, carbonization ~ vermiculite : 氧 Oxygen (4), carbonaceous materials such as graphite, carbon fiber, talc pigment, Ming particles, stainless steel particles, bronze particles +, copper / word = pull, copper / chrome alloy particles. Can be used as an infrared light-shielding substance The above-mentioned metal particles or non-metal particles may be used alone or in combination of two or more. As the infrared light-shielding particles, particularly preferred are cerium oxide, cerium citrate, titanium oxide or cerium carbide. The composition of the infrared light-shielding particles can be obtained by FE_SEM EDX. (Field Emission-Scanning Electron Microscopy Hnergy-Dispersive X-ray Analysis, field emission type scanning electron microscope energy dispersive X-ray analysis). The average particle diameter of the infrared light-shielding particles is 200 ° C or higher. From the viewpoint of heat-dissipation performance, it is preferably 〇. 5 μπι or more, and the heat-dissipating property at a temperature of less than 2 〇〇t is obtained by solid conduction conducted by 158675.doc -27-201228989 From the viewpoint of the above, it is preferably 30 μη or less. Further, the average particle diameter of the 'infrared light-shielding particles can be obtained by the same method as the cerium oxide particles or the alumina particles. The average particle diameter of the infrared light-shielding particles is also affected. The influence of the size of the inorganic fibers, the cerium oxide particles, and the alumina particles is such that the cerium oxide particles and/or the aluminum oxide particles are in the range of 5 nm to 100 μΓΠ2, and the infrared ray is easy to be used. The inventors of the present invention have found that the average particle diameter of the mixed-capacity particles of the alumina particles is preferably 〇5 or more preferably 0.5 μm or more and 5 μηι or less. The infrared reflection, scattering, or absorption efficiency tends to depend on the volume ratio of the infrared light-shielding particles contained in the heat-insulating material. The content of the infrared light-shielding particles in the heat-insulating material is preferably based on the volume of the entire heat-dissipating material. 〇% by volume and 5% by volume or less. If the content of the infrared ray-shielding particles is more than 5% by volume, it is transmitted by solid conduction. The heat is large, so there is a tendency that the heat-breaking performance is lower at a temperature of less than 2 ° C. In order to improve the heat-breaking performance at the above temperature, the content of the infrared light-shielding particles is more preferably 〇. 5% by mass or less, and more preferably 〇〇3 body (four), or 4 vol% or less. The above-mentioned 为 is 6 〇 mass% or more, and the amount is less than or equal to the range of The powder of large particles and the mixed powder of infrared light-shielding particles tend to be less hygroscopic, and have the effect of less uniformity during weighing. In addition, 'the presence of dioxin-cut particles and/or oxidation in the non-Lu particles and infrared (IV) The (four)-increasing (four) tendency of light particles is difficult for the sand mixer or the mixing machine to disturb the mixing tank and the mixing tank. It has the capacity of 158675.doc •28· 201228989 particle p degree/knife loose mixing state, mixed The effect of less recovery loss of the powder. When the infrared light-shielding particles are set with respect to the powder. Above .lft%, quality - below, there is capacity:::: = light: the content of the sub-content is set to exceed. The tendency to be 5% by volume and not more than 5% by volume is more preferably 〇5 mass% or more and 35 mass% or less, and still more preferably 1 mass% or more and 30 mass% or less. For example, the composition of the infrared light-shielding particles can be determined by using the FE_SEM edx, and the element contained in the infrared-only particle can be quantified by the glory X-ray analysis method. . [1-4] Thermal Conductivity The thermal conductivity of the heat-insulating material of this embodiment is 0.05 w/m·K or less. From the viewpoint of heat-dissipation performance, the thermal conductivity state may be _Z, preferably 〇.045 w/m.Kay, more preferably _W/m·K or less, and thus better A η" Below °·037 W/m · K, the best is 〇.〇237 W/m.Km. In particular, when the heat-dissipating property in the above high-temperature region is required, the heat-insulating material containing the infrared light-shielding particles is preferable. When the powder contains infrared light-shielding particles, the thermal conductivity at 8 〇〇t is preferably 0.2 W/m.K or less, more preferably 〇19 w/m.K or less, and even more preferably 〇18 W/m.K or less. The method of measuring the thermal conductivity will be described later. When a plurality of kinds of cerium oxide particles and/or oxidized particles, for example, small particles and large particles are mixed to prepare a heat-insulating material, it is preferable that R1 is 60% by mass or more and 9% by mass or less. The heat-insulating material is prepared by containing small particles and large particles (4) to fix heat (4). When the thermal conductivity exceeds the clear form of I5 I38675.doc •29·201228989, it is preferred to change the mixing ratio within the range of maintaining the above content ratio. When inorganic fibers or infrared light-shielding particles are used, the amount of mixing can be determined in the same manner. When the mixing ratio of the inorganic fibers and the infrared ray-shielding particles is excessive, the heat-dissipating property may be lowered. Therefore, it is preferable to carry out the measurement while confirming the thermal conductivity. For example, when the average fiber length of the corpus callosum is 12, and the average length of the inorganic fibers is 靡, the mixing ratio of the inorganic fibers is preferably ≥ mass% or less. For example, in the case of -oxidation; in the case of mixing the infrared light-shielding particles having an average particle diameter of 2 (four), the mixing ratio of the infrared light-shielding particles is preferably ≤ mass% or less, and the right is selected from a material having a small thermal conductivity. In the inorganic fiber or the infrared light-shielding particle, there is a tendency to easily prepare a mixed powder having a thermal conductivity of 〇〇5 w/m·κ or less. [1-5] BET specific surface area 2 The heat insulating material of the present invention has a BET specific surface area of 5 m 2 /g or more and 15 〇 m 2 : g or less. The heat-insulating material having the BET specific surface area in the range tends to have a tendency to store the heat-dissipating material or to agglomerate in the supply step of the mold, to suppress the flying at the time of molding or at the time of filling, and to have a small thermal conductivity, so that it is preferable. . The method for measuring the BET specific surface area will be described later. When the BET specific surface area is 5 m 2 /g or more and 15 μm 2 /g or less, and further contains small particles including ceria and/or alumina and having a particle diameter of Ds & 5 or more and % nm or less, formability exists. Excellent, the powder is less scattered, and the heat-dissipating performance tends to be excellent. The reason is not clear, but it can be speculated as follows. Small particles having a particle diameter Ds of 5 nm or more and 30 nm or less are previously easy to aggregate, and loose bulk density is small, and is easily scattered. With respect to I58675.doc -30-201228989, a method of mixing small particles with the above-mentioned large particles as a method of adjusting the BET specific surface area to 5 m2/g or more and 150 m2/g as the above-mentioned small particles is used. It is presumed that if the heat-insulating material is adjusted in such a manner, the property of easy aggregation of the small particles causes the large particles to adhere with moderate strength, and as a result, the scattering of the powder is suppressed. Further, small particles tend to aggregate when stored, and it is presumed that one of the causes is that the powder-like heat-insulating material containing small particles has a large BET specific surface area, so that it is easy to absorb moisture in the air. On the other hand, it is estimated that by adjusting the BET specific surface area to 5 m 2 /g or more and 150 m 2 /g or less, the absorption of moisture in the air can be suppressed, and the powdery heat-insulating material becomes less likely to aggregate. Preferably, it is 5 m2/g or more and 130 m2/g or less, more preferably 1 〇m2/g or more, 115 仏 or less, and further preferably 15 m2/g or more and 1 〇〇m2/g or less, particularly preferably 2〇m2/g or more and 91 m2/g or less. [1-6] The content of the metal element, the earth metal element, the Ge, p, j?e, the powder of the present embodiment preferably contains an alkali metal element selected from the viewpoint of suppressing the scattering of the heat insulating material. At least one element selected from the group consisting of alkaline earth metals and strontium. Specific examples of at least one element selected from the group consisting of an alkali metal element and an alkaline earth metal element (hereinafter, referred to as "initiative element" in the present specification) include lithium, sodium, unloading, and hydrazine. Alkali metals such as planing, alkaline earth metals such as magnesium, calcium, strontium and barium. The basic element □ is only one type, and may contain two or more types. The type thereof is not particularly limited, and it is preferable to improve the adhesion of the particles to each other, or to perform hardening by heat treatment at a relatively low temperature, and it is preferable to carry out the work, the unloading, the money, and the mother. l:58675.doc -31 - 201228989 When the heat-dissipating material contains an alkaline element, the content of the basic element is preferably 〇. 5% by mass or more, and 5 mass based on the total mass of the heat-dissipating material. When it is contained, it is preferably 1 〇 mass ppm or more and 1000 mass ppm or less, and the content ratio of p is preferably 〇〇〇 2 mass % or more and 6 mass % or less.

The content of Fe is preferably 〇〇〇5 by mass. /〇 or more, 6 mass% or less. Further, the content of P is preferably 0 002. / ((above, 6% by mass or less. In addition, from the viewpoint of improving adhesion or fluidity of particles and suppressing aggregation, it is more preferable that the content of the basic element is 〇〇〇5% by mass or more and 3 masses) % or less, the content ratio of Ge is 20 mass ppm or more and 900 mass ppm or less 'the content ratio of P is 0.002 mass. /〇 or more, 5.5% by mass or less, and the content ratio is 0.005 mass. The content of the test element is preferably 0.005 mass% or more, and the content of the test element is 20 mass ppm or more and 8 mass ppm or less, and the content ratio of p is 0.002. The content of Fe is not less than 5% by mass and not more than 5% by mass, and the content of Fe is 〇.0〇5 mass 0/. or more and 2 mass%/〇. The content of basic elements, Ge ' P, and Fe in the heat-insulating material may be Quantitatively determined by XRF (fluorescence ray ray analysis). If an alkali metal element, an alkaline earth metal element, or Ge is contained in a large particle, the scattering or aggregation of the heat-insulating material is suppressed, and the productivity is improved when the heat treatment is performed. Significantly appearing, so it is better. The basic element or Ge, P, Fe of the content of the above-described method may be, for example, by utilizing the separated large particles and small particles, determined using the fluorescence was measured χ-ray analysis. [I-7] Compressive strength

158675.doc 32 S 201228989 The formed heat-insulating material of the present embodiment is less likely to be collapsed or deformed during compression, and it is possible to perform shape processing such as cutting without causing collapse, and has a heat-dissipating property. The maximum load in the range of 〇 5% to 5% is 0.7 MPa or more. More preferably, it is 2. MPa or more, and more preferably it is 3 〇 MPa or more. The upper limit of the maximum load in the range of the compression ratio 〇 5% is not particularly limited. From the viewpoint of the heat-dissipating performance, 3 〇 MPa or less is suitable. The compression ratio can be calculated from the stroke (pressing distance) of the sample thickness at the time of measuring the compressive strength, that is, the length of the sample in the compression direction. For example, when the compression strength is measured by using a sample obtained by forming a molded body into a cubic shape of 1 cm x 1 cm x 1 cm, the state of the stroke of 〇·5 mm is defined as compression: 5%. The compression ratio can be calculated by the following formula (1). Compression ratio = 100x stroke (pressing distance) / length of compression direction of the sample (1) The pattern of the load-compression ratio curve drawn when the compressive strength is measured is not particularly limited. That is, in the range where the above-mentioned compression ratio is 〇 to 5%, the molded article of the sample collapses and shows a clear breaking point, or does not collapse. In the case where the compression ratio is 0 to 5%, the molded body collapses as a sample. i: In the case of a crack, the maximum load of the molded body is defined as: crack: load. The load at the breaking point is preferably 〇 7 Μ ρ & or more, and is more than 2 MPa, and more preferably 3 QMpa or more. When the sample is not (4) = 〇, the maximum value / displayed in the range of the compression ratio 〇 ~ 5% is used. The value of the compressive strength can be measured by the method described later. Π-8] Cumulative micropore volume l:) 8675.doc -33· 201228989 In the formed heat-insulating material of the present embodiment, the cumulative micropore volume ν of the pores having a pore diameter of 0.05 μm or more and 0.5 μηη or less The ratio r is preferably 70% or more of the cumulative micropore volume V〇.〇〇3 of the micropores having a pore size of 0·003 μm or more and 150 μηη or less. R can also be expressed as (γ·/ν〇.〇〇3)χΐ〇〇. The larger r is, the narrower the micropore distribution is. The pore size is concentrated in the range of 〇〇5 μmη or more and 〇5 or less. As a micropore distribution of a heat-insulating material having a R of less than 70%, the following cases are conceivable: 〇) a case where a plurality of pores having a pore diameter of less than 〇〇5 are present in the formed body; and (2) a majority of pores in the formed body exceed 〇 5 micro. The case of the hole; (3) There are micropores having a pore diameter of less than 5 μm and more than 0.5 μηι in the molded body, and there are few micropores of 0.05 μm or more and 〇5 μm or less. In the case of (1), there is a tendency that the heat-dissipating material tends to collapse into a powder form when wetted by water (liquid), and in the case of (7), there is a tendency that the heat-dissipating property is low, and (3) In the case, the tendency of (1), (2) appears depending on the ratio of various apertures. If ν〇 〇5 is less than 5 mL/g, the heat-dissipating performance tends to be low, and if it exceeds 2 mL/g, it tends to collapse into a powder form when wetted by water (liquid). Furthermore, the preferred form is 5n^2·5 mL/g or less. The reason is not clear, but it can be inferred that (2: when wetted by water, 'the contraction force is generated by the capillary phenomenon, the particles forming the void move, etc., and strain occurs in the heat-dissipating material, and the shape 1 is broken (7). Unexpectedly, since the pore diameter is larger than the air molecule, that is, about 1 GG nm, the convection by the air or the conductive 敎 material m is difficult to be suppressed, and the heat-dissipation performance is degraded. : From the viewpoint of collapse and powder formation during humidity control, the total pore volume of the crucible is more preferably 75% or more, and is 158675.doc -34 - 201228989 8〇% or more. Loo%. The pore size is 〇.〇5 μηι or more, and the i5 product % is preferably 〇.5—above, 2 mL/g^ the cumulative micropore volume of the pores by the following: ^I tired micropore volume/ The value measured by the mercury infiltration method is defined. It is inferred that within the above range, the heat-dissipating material has a moderate thermal insulation performance. v〇.G5 is preferably 0.5 mL/g or more, 丨7, 5 丄L7 It is more than mL/g, and more preferably 〇.5mL/g or more, and is - below. Further, it is preferably 55mL/g or more, 2.5_ or less, more preferably 0.5mL. / g or more, 2 mL / g or less, more preferably 〇 6 mL / g or more, 2 reddening or less. 1.2] Method of manufacturing the heat-insulating material The method of manufacturing the heat-insulating material of the present embodiment includes the following steps: a small particle containing cerium oxide and/or aluminum oxide and having an average particle diameter of 5 nm or more and % or less, and containing cerium oxide and/or aluminum oxide, and having an average particle diameter of 50 nm or more and 100 μm or less In the large particle, the ratio I of the mass of the large particle to the total mass of the small particle and the mass of the large particle is two masses / 〇 or more and 90 mass % or less, and is mixed as a heat-insulating material. Preferably, the method comprises the steps of: arsenic trioxide and/or aluminum oxide, and small particles having an average particle diameter of 5 nm or more and 30 nm or less, containing cerium oxide and/or aluminum oxide, and being selected from alkali At least one of a group consisting of a metal element, an alkaline earth metal element, and lanthanum, and a large particle having an average particle diameter of 50 nm or more and 100 μm or less, with a mass of the large particle relative to the mass of the small particle and a large particle The ratio of the total mass of quality R L is 60% by mass or more and 90% by mass or less to obtain an inorganic mixture. 158675.doc -35- 201228989 In the method for producing the above-mentioned heat-insulating material, in terms of thermal conductivity, small particles The average particle diameter is preferably '25 nm or less on nmu, more preferably 5 nm or more and 20 nm or less', and more preferably 5 nm or more and 18 nm or less 'excellently 7 nm or more 'I4 nm or less. It is known that the particle 'large particle is used as a raw material for the heat-insulating material for the sake of simplicity'. When using commercially available small particles, large particles, and the average particle size indicates the shape of 愔&, this value can be regarded as the average particle diameter of each particle." The particle size of the commercially available product - Μ Μ -'01 - There are various methods for the He ^ Chuanxiong method. It is also possible to determine the diameter of the method. However, according to the usual measurement method, the method has a thousand-average particle size of 5 nm or more and 30 nm & There are a plurality of small particles having a particle diameter of nm or more and 30 nm or less: the average particle diameter of the large particles does not cause a difference in the degree of the heat insulating material. Therefore, there is no problem. When the average particle size of the raw material is unknown to you, the average enthalpy of the small particles can be assumed to be spherical. The following formula (4) measures the specific surface area of the small particles 'by d=6/ps (where d is the particle) The diameter [m], 2 r , 3 ” horse specific surface area l > /g], p is the dense sound [g/cm3]). When the temperature is not spherical, the average particle size may be 5 nm or more and 30. However, even in this case, if the diameter is 5 (10) or more and 3 〇 or less, it does contain a plurality of pines. There are no problems with small particles below the width. The measurement method can be carried out using nitrogen as the adsorption gas (nitrogen absorption). The BET method is used for the surface area. For example, the gas can be used for the measurement. 158675.doc

S • 36 - 201228989 Adsorption measuring device (Autosorb 3MP, manufactured by Yuasa Ionics &amp; Division). The density P [g/cm ] refers to the true specific gravity determined by the pycnometer method. As the measuring device, for example, an automatic wet true density measuring device (Aut〇 True MAT-7000, manufactured by Seishin Enterprise Co., Ltd.) can be used. The average particle size of the large particles can also be determined in the same manner as the small particles. In the method for producing the heat-insulating material, the average particle diameter of the large particles may be 80 nm or more and 1 μm or less, but if it is 5 〇 nm or more and % _ or less, the heat-insulating material contains inorganic fibers or Infrared shading grain? When the crystal is uniformly mixed with the above, it is preferable. When it is 5 〇 (10) or more and ι ’ or less, the adhesion of the particles is large, and the particles are less taxed from the powder. Therefore, it is more preferably 5 Gnm or more and 5 μm or less. 1 The ratio of the mass of the large particles is preferably 6 〇 mass% or more, Μ mass% or less, more preferably 65 mass% or more, 8 mass% or less, and still more preferably 65. The mass% or more and the 75 mass% or less. The following steps. It is to be noted that the raw materials used in the method for producing the heat-insulating material and the ruthenium-containing particles, the alumina particles, and the oxidized (four) sub-processes each contain a dioxane component, and the particles can be made small particles and large. The mixing ratio of the particles, &lt;·&quot;, and the conductivity are adjusted. For example, the wet method under the oxidizing condition makes the acid-breaking acid: the fineness is determined by the acid or the tester, and the hydrolysis and condensation are carried out for the bismuth fossil component produced by the wet method: 58875 .doc •37· 201228989 2:: It is also possible to burn a compound such as a vapor in the gas phase. - The oxidized stone particles can also be produced by oxidizing and burning the gas of the Shishi metal or the stone of the original stone. The cerium dioxide particles may also be prepared by melting vermiculite or the like to produce i ^ 趟 趟 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 The aluminum particles can also be processed by the Bayer method (Bayer pr〇 - obtained "Bayer based on gibbsite or soft water sorghum nme" as the raw material '(4) sodium hydroxide treatment principle, also It can be used to treat Shaoshui Sanshui, soft water, purified miscellaneous stone (dlaSP〇re), and point soil 'Ming Xinshi with sulfuric acid, such as sulfuric acid, etc. The acid group is separated, and each of the cerium oxide particles or the aluminum oxide particles may contain cerium oxide. The component other than the cerium lanthanum is exemplified as the above-mentioned production method: it is present in the raw material as an impurity. A method for producing a known cerium oxide to which a component other than cerium oxide or oxidized cerium is added in the production process is as follows. <The cerium oxide synthesized by a wet method> The gel method of the raw material is made of acidic gel dioxide. The sodium sulfate is prepared as a raw material for the readability of the dioxide dioxide. The dioxide synthesized by hydrolysis and condensation of dioxyl money. Synthetic cerium oxide by dry method&gt; The sulphur dioxide produced by the burning of the sulphur dioxide. The sulphur dioxide is obtained by vaporizing and oxidizing the metal at a high temperature. 158675.doc

S •38- 201228989 二 β 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽 矽The pulverized cerium oxide powder is melted in a flame and spheroidized to obtain a melting. The manufacturing method of the well-known Oxide Ming has the following methods. Alumina obtained by an acid method. Alumina obtained by the Bayer process (alkali method). The calcined alumina obtained by granulating, drying, and calcining the calcined alumina produced by the Bayer process. An fused aluminum oxide obtained by melting a raw material in an electric furnace and then crystallizing and solidifying. A white fused alumina using pre-fired alumina produced by the Bayer process as a raw material. Brown fused alumina with bauxite as the main raw material. Smoked and oxidized. An alumina obtained by vaporizing and oxidizing a metal at a high temperature. Among the dioxodes obtained by the respective production methods, the method of making acid by using Reiner as a raw material: oxygen (4), and the deposition method of dioxotomy by using sodium as a raw material The cerium dioxide synthesized by hydrolysis and condensation of money, which is produced by burning the chloride of cerium, and the cerium oxide produced by burning the cerium metal gas, by the arc method or the plasma method In the production of the sulphur dioxide, it is easy to cause formation defects and tend to be scattered and easily aggregated. By mixing the average particle diameters in the above-mentioned manner, I58675.doc -39-201228989: formation defects or scattering, agglutination, and therefore preferably also obtained by using other methods & methods A plurality of oxidized particles or alumina particles of the cerium oxide particles or the oxidized particles are mixed. ^Make the material M w ash, so that the pulverized d-cut powder is melted in the flame and spheroidized to obtain the molten sulphur dioxide, obtained by the Bayer method, sintered oxidized, electrofused oxidation (white fused oxide) The thermal conductivity of brown electric refining oxidation exceeds 〇.〇5 w/mK. Therefore, only the raw material obtained by the manufacturing method, or the oxidized sulphur, is used as the raw material of the dioxide dioxide In terms of rate, it is not preferable. It is excellent in terms of operation. It is also sometimes useful in terms of cost. Because it can be obtained by mixing and using other manufacturing methods: Γ conductivity is adjusted to °·°5 w/mK or less, and therefore (4) η. When alumina or the like is used as a raw material, it is preferably a dioxide granule obtained by the method of its production: ° - : smoked by the burning of the chloride of the stone Oxide oxide, the stone eve: the body is burned to produce the oxidized stone, the smoked oxidized sulphur-containing ash, sintered alumina, etc. The oxygen conductivity of the package is reduced by the ionic particles and/or alumina particles. :=:=, in the case of productive Μ - the oxidized ash ashing r metal gas is burned Alumina, sintered alumina obtained by the ear method. Natural mineral acid minerals can be used from the worship particles. As a mineral of the day, for example, acupoints, olive stones, and olivine stones, Quartz, length 158675.doc 201228989 Di-zeolites, etc. As a substance of oxidized granules. Natural minerals of oxygen ^ can be enumerated: Mingtian days ^ = can be used as synthetic mullite) Moco by natural minerals Cheed her from the electric stone. As the oxidized "sub-particles of the powder", the [2-2] alkali metal element, alkaline earth metal element, Ge, P, and Fe are used in the production process of the oxidation oxidation process or the heat-dissipating material. System: Two-part bismuth contains the basic element -, ... the shape of the compound: Two: 'It is also possible to pre-contain a sufficient amount of the test element, Ge, p, Fe, and/or oxidized particles as the raw material of the heat-insulating material. Γ: The compound of the second check element 'Ge, p, Fe, which is not particularly limited to oxides. 'Alkaline elements, Ge, p, oxides, complexes, hydroxides, nitrides, carbides, carbonates Salt, acetate, 2 salt, salt, poorly soluble salt, and hospital oxide. These may be used alone or in combination. The inorganic compound particles containing the inorganic compound particles containing the intrinsic element ", ep, and Fe as impurities" are used as raw materials of == in terms of productivity, cost, workability, and the like. The inorganic compound particles of the ruthenium can be obtained, for example, from the ash of a by-product such as the particles of the dioxo-cut gel produced by the shoji method. The method of the compound of P and F4 is obtained, for example, by adding to the above-mentioned wet method or dry method, one of the cerium oxide, the alumina obtained by the acid method or the alkali method, and the sintering. 158675.doc -41- 201228989 In the electro-oxidation oxidation, it can also be added in the above-mentioned steps of dioxo-cut or oxidized neon. The chemical substances containing alkaline bismuth P and Fe can be water-soluble. It may be insoluble in water. It may be added in the form of an aqueous solution of each of the compounds (4), &amp;, and: and may be added in the form of a solid or liquid as needed to contain an inspecting element, e P, Fe. a compound of each of them. It contains a basic element &amp; Laid previously pulverized to a coarse grinding. Further Laid ... 'may pre-advanced

Ge ' p cerium oxide particles or alumina particles contain an excessive amount of basic elements, and can be used in the manufacturing process of cerium oxide or the production of powder: a certain treatment is applied, and the content of the above elements is Adjust to special =: method IS test, ", _ to specific range: ^ enumerate the amount of substitution using acidic substances or other elements;: whole: in addition to the method 笙, thousand tongue or aqua regia, etc., including cerium oxide The inorganic compound particles are contained in nitric acid and used as a raw material for drying. The inorganic compound particles of the desired particles are pulverized to a desired excess of the basic element, Ge. , P, Fe, can also be alkaline 7L, G force J in fossil ray particles. P, Fe adjusted to a specific range, pulverized diox [2-3] mixing method, a oxidized stone slab early machine The fiber can be mixed with human oxygen ray particles, infrared light-shielding particles, and the 6th edition (Maruzen &amp; Known Powder Mixer, for example, the Chemical Engineering Handbook). In this case, you can mix 2 kinds to 158675. Doc

In S-42·201228989, the inorganic compound particles containing the cerium oxide may be mixed, and a compound containing the test element, Ge, P, and Fe or an aqueous solution thereof may be mixed. In the known powder mixer, as the container rotation type (rotation, vibration, and movement of the container itself), a horizontal cylinder type, a V type (which may be accompanied by a transfer blade), a double cone type, a cubic type, and a swing are exemplified. Rotary type; as a mechanical drop type (container fixed, stirring with a blade, etc.), it can be exemplified by a single shaft belt type, a double shaft stirring type, a rotary coulter type, a double line money type, a _ spiral type, a high (four) type, Rotating disc type, rotating container type with roller, rotating container type with mixing, high-speed elliptical rotor type; as flow (four) type (using air, gas: stirring), airflow stirring type, gravity Non-mixing type. Also = use this special mixer in combination. The mixing of the cerium oxide particles and/or the aluminum oxide particles, the infrared ray opaque particles, and the ruthenium-free fibers can be used as a pulverizer. For example, the pulverized particles or the cuttings described in the 6th edition of the Chemical Engineering Review Revision (Maruzen) Inorganic fiber, which enhances the dispersibility of particles or inorganic fibers, and mixes them on the surface. In this case, two or more kinds of cerium oxide particles and/or alumina particles may be pulverized and dispersed, and may be pulverized or dispersed to contain an alkaline element, Ge, p,

A compound of each of Fe or an aqueous solution thereof. As a known pulverizer, a roll mill (high pressure compression roll mill, roll type barrel mill), a masher, a rim machine (a double-axis rim machine (fret mill), a Chilean rim machine) (chnean_ mill)), cutting/shearing mill (cuUer mm, etc.), rod mill, self-grinding machine (air drop type self-grinding machine (aer0fall min), waterfall type self-grinding machine ( Cascade mill), vertical roller mill (ring mill, roller-race mill, ball-race mill), high-speed barrel grinding '-58675. Doc •43- 201228989 Machine (hammer mill, cage mill 'dry mill' screen mill, disc pin mill), classifier built-in high-speed barrel mill (fixed impact plate mill 'turbine mill Machine, centrifugal graded plastic grinding machine, ring mill), container driven medium grinding machine (drum type ball mill (can grinder, tube mill 'conical ball mill), vibrating ball mill (round vibrating mill, rotary vibrating mill, Centrifugal mill), planetary mill, centrifugal flow mill), medium agitating mill (tower mill, stirred tank mill, horizontal flow tank) Mill, vertical flow channel mill, ring gap sander), airflow mill (air flow insertion type 'nozzle pass type, collision type, fluid layer jet blow type'), compacted shear mill Machine (high-speed centrifugal grinding machine, inner stator (i_r piece) type), material, stone grinding, etc. These pulverizers can be used in combination. Among these mixers and pulverizers, a powder mixer with a stirring blade, a high-speed barrel mill, a classifier built-in high-speed (four) machine, a container-driven media mill, and a compacting shear mill can lift particles or inorganic fibers. Dispersibility is therefore preferred. In order to improve the dispersibility of the particles or the inorganic fibers, it is preferable to set the peripheral speed of the front end of the rotating blade, the new plate, the blade, and the pin to 100 km/h or more, which is more than a helmet. 2 〇〇 _ or more, and more preferably _ mixed plural kinds of cerium dioxide emulsified scorpion and / or alumina particles ' ' 'better in accordance with the volume ratio will be white and ^ i A order will be three The oxidized stone granules or oxidized |g particles are put into the picking 撼+ &amp; picker or pulverizer. In the case of a right-handed fiber or an infrared light-shielding particle, after the particle and/or the oxidized particle, it is preferred to mix the dioxide, then add the inorganic fiber and mix. Line-preserving particles and 158675.doc 201228989 [2-4] Forming method The forming step of forming the inorganic mixture in the present % form may be (a) ~ surface pressing the inorganic mixture with a forming die, heating to 400 ° The step C or more may be a step of (b) forming the inorganic mixture by pressurization and then performing heat treatment at a temperature of 400 C or higher. In the forming step, it is preferable to set the molding pressure so that the bulk density of the heat-insulating material is 0.25 g/cm3 or more and 2. 〇 g/cm3 or less. Further, the manufacturing method of the present invention comprises: a forming step of forming the inorganic mixture '(4) step 'cutting a part of the formed body obtained by the forming step; and the forming step may be (4)-face to make the formed heat-insulating material The step of heating the pressurizing surface of the inorganic mixture by a forming die in a manner of a density of 0,25 g/cm 3 or more and 2 〇g/cm 3 or less, or (4) adding the inorganic by using a forming die After the mixture is formed, the heat treatment step is carried out at a temperature of 400 ° C or higher. In the case of a powdery heat-dissipating material, it may be directly used by filling a powder-like heat-insulating material in a use portion without undergoing a step such as forming, or may be used to pressurize the powder-shaped heat-insulating material. The molded product is used as a heat-insulating material. When a powdery heat-insulating material is press-formed to produce a molded body, it can be formed by a press molding method (piston type press molding method), a rubber pressing method (hydrostatic molding method), or an extrusion molding method. It is shaped by a conventional press-forming method known in the art. In view of the productivity of the 龅 旺 , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , , It is preferable to apply a vibration or the like to the powder-shaped heat-insulating material to uniformly fill the thickness of the molded body. When the powdery heat-breaking material is filled into the mold while being decompressed and degassed in the mold, it can be filled in a short time, and therefore it is preferable from the viewpoint of productivity. The bulk density of the obtained molded body is preferably set to be 0 25 g/cm 3 or more and 2 〇 g / cm or less from the viewpoint of reducing the load during transportation. If the molding conditions are to be controlled by the pressurizing pressure, the sliding property of the powder-like heat-insulating material to be used, the amount of air introduced between the particles of the powder or the micropores, and the like, In the state of holding the time, the pressure value changes, so that production management becomes difficult = tendency. On the other hand, the method of (4) bulk density can be easily made to achieve the target value of the obtained molded body without controlling the time. The bulk density of the formed powdery heat-insulating material is preferably 〇g/cm3 or more and 1.7 g/cm3 or less, and more preferably 〇g/cm3 or more and 1.5 g/cm or less. The bulk density of the bulk is 〇25 g/cm3 or more, and the forming pressure of 2.〇g/cm3 or less is, for example, a pressure slightly equal to or greater than 〇〇1 and a pressure of 50 MPa or less. 25 or more The forming pressure of 'l_7g/cm3 or less, for example, 〇〇1 Μρ&amp; above, pressure below 4〇Mp, as the forming pressure at a bulk density of 〇.25 g/cm3 or more and i 5 g/c^a 'For example, _ slightly above' 3G Μρ &amp; the following pressure. Further, the bulk density of the formed heat-insulating material is calculated by measuring the size and mass of the heat-insulating material in the form of the heat-dissipating material. For example, in the case where the heat-insulating material has a layer structure, it is not measured only in its specific use density, but in the state of the actual use form, that is, the layer structure: I58675.doc -46 - 201228989 Size and quality. If the bulk density is not changed by processing such as cutting, the heat-insulating material can be formed into a size that is easy to measure and the bulk density can be measured. An example of a method of producing a heat-insulating material in such a manner that the bulk density of the obtained heat-insulating material is a specific size will be described. First, the weight of the desired inorganic mixture is determined based on the volume and bulk density of the heat-insulating material. Then, the weighed inorganic mixture is filled into a forming mold to be formed by pressurization in such a manner as to form a specific thickness. Specifically, in the case of producing a molded body having a length of 30 cm, a width of 30 cm, a thickness of 2 mm, and a bulk density of 0.5 g/cm 3 , the bulk density of the target can be made by the molded body to be produced. The volume is multiplied to determine the weight of the powder required to make the heat-insulating material. That is, in the above example of the heat-insulating material, 〇5 [g/cm3] x 30 [cm] x 30 [cm] x 2 [cm] = 900 [g], and the desired powder is 900 g. In general, in the case of producing a molded body having a volume of a cm 3 and a bulk density of β g/cm 3 (where β is larger than the loose bulk density of the powder), by weighing only the powder of αβ g , And the powder is compressed, and can be formed into a volume of 0: 〇 if the powder-shaped heat-dissipating material, or the heat-dissipating material after press forming or press forming, the powdered or shaped heat-dissipating material It is preferable to heat and dry in a range of temperature or time conditions sufficient for heat resistance to remove the adsorbed water of the powdery or formed heat-insulating material and then supply it to practical use, since the thermal conductivity is low. Further, heat treatment can also be performed. The molding may be carried out only by press molding, and it is preferred to heat-treat the person who is subjected to press forming. When the heat treatment is carried out on the person who press-forms the powder, the compression strength is improved, and it can be suitably used for applications having a large load. Just improve 158675.doc -47- 201228989

From the viewpoint of the heat treatment step, it is preferable that the ruthenium metal element, the alkali 3 metal element, and the Ge, P, and Fe' are contained in the large particles in the powder. From the standpoint of dimensional stability, the heat treatment temperature is preferably a temperature higher than the highest use temperature of the body-shaped or red-formed heat-insulating material. The heat treatment 'the degree of the dish is also various depending on the use of the powder or the formed heat-dissipating material. Specifically, it is preferably the top, the 1400 tM = preferably 500 C or more, 13 G (the following is better than rc) 1200 ° C or less. The environment of heat treatment of the shape or shape of the heat-dissipating material can be enumerated. = medium (f atmosphere), oxidizing environment (oxygen, ozone, nitrogen oxidation f - fossil reaction, hydrogen peroxide In the environment of hypochlorous acid, inorganic/organic peroxides and inert gases (environment, gas, gas, nitrogen, etc.), it is also possible to add water to the environment...heat treatment time as long as it is based on heat treatment temperature and heat The amount of the material may be appropriately selected. The heat treatment may be carried out after the powder material is filled in the use site, or may be applied to the powder heat-pressing material. The heat-dissipating material covering material having the outer material is preferably a heat-insulating material containing powder and/or containing powder, and a material for containing the outer material. The coated body is in the form of a powdery heat-breaking material or a formed heat-dissipating material. , (Iv) easy 'the advantages of easy construction also Furthermore, sometimes accommodated in the outer heat insulation material is referred to as the core material., The material is I58675.doc [3-1] outer

S • 48· 201228989 The material to be used is not particularly limited as long as it is capable of accommodating the powdery material and/or the formed heat-dissipating material as the core material, and examples thereof include glass cloth, oxon fiber cloth, and Inorganic fiber woven fabric such as oxidized stone sap, inorganic resin needle, resin film such as polyethylene, polypropylene film, nylon film, poly-p-phenylene film, fluorine resin film, etc. , aluminum, stainless steel y!, copper falling and other metal falling, ceramic paper H fiber non-woven ^ organic fiber non-woven fabric, glass fiber paper, carbon fiber paper, rock thief paper, ..., machine-filled paper, organic fiber paper, ^ porcelain coating Resin coatings such as layers, fluororesin coatings, and epoxy resin coatings. In terms of reducing the heat capacity of the special (four), the thickness of the outer material is preferably thin, and may be appropriately selected depending on the use condition or the strength required. When the material to be coated is formed of a material which is stable at the temperature at which the core material is used, it is also used as a powder material of the core material and/or a heat-dissipating material which is formed as a material for the outer material. ^. In the case of a covering used at a high temperature, it is preferable to use a material having a high heat resistance from the viewpoint of easy handling of the core material. In the present specification, the "outer material" is divided by m. In addition to the core material, it is also included in the handling of the core material or the construction of the core material. That is, the outer material includes the core material only during transportation or during construction, and is melted and/or volatilized during use, so that the outer material or the organic component contained in the outer material is melted at the use temperature of the core material. Or disappear. The outer cover material is preferably in the form of a sheet such as glass cloth, oxidized fiber cloth, sulphur dioxide cloth, inorganic fiber woven fabric, inorganic fiber woven fabric, polyester, and the like. Membrane, polyethylene touch, polysilicon film, nylon film, polyethylene terephthalate film, fluorine resin film, etc. 158675.doc -49- 201228989 Resin film, plastic-metal film, steel box, stainless steel thread, Metal enamel such as copper box, ceramic money, inorganic fiber non-woven fabric, organic fiber non-woven fabric, glass fiber paper, carbon fiber paper, rock, velvet paper, inorganic filler paper, organic fiber paper. When the covering is used at a high temperature, the outer material is more preferably an inorganic fiber woven fabric such as glass cloth, oxidized fiber cloth, or oxidized stone cloth, or inorganic fiber knitted fabric from the viewpoint of thermal stability. Paper, inorganic fibers are not woven. From the viewpoint of strength, the outer material is more preferably an inorganic fiber woven fabric. Method of coating material other than [3 - 2 ] Powder-type heat-insulating material may contain cerium oxide particles and/or alumina particles, and may contain large particles 'infrared opaque particles or inorganic fibers depending on the use conditions. The formed powder is filled as a core material in a material which is processed into a bag shape or a tubular shape, and may be a material which is formed by press molding the powder and is used as a core material. In the case where the powdery heat-insulating material is used as the core material, the filling rate of the volume formed by the powder with respect to the outer material can be appropriately set depending on the object using the powder-shaped heat-insulating material. In the case where the formed heat-dissipating material is used as the core material, as described later, the powder-shaped heat-insulating material may be press-formed together with the outer material, or the powder-shaped heat-insulating material may be used. It is covered with a material other than after press molding. The method of coating the core material with the material other than the material is not particularly limited, and the preparation or molding of the core material and the coating of the foreign material may be simultaneously performed, or the material may be coated after the core material is prepared or formed. The outer material is inorganic fiber woven fabric, resin film, plastic-metal film, metal foil, ceramic paper, inorganic fiber non-woven fabric, organic fiber non-woven 158675.doc •50· 201228989 cloth, fiberglass paper, carbon fiber paper, rock wool In the form of a sheet such as paper, inorganic filler paper or organic fiber paper, for example, it can be coated by using an inorganic fiber yarn or a resin fiber yarn, followed by fixing the outer material ', and sewing and then coating. In the case where the outer material is a resin film, a plastic film, a metal foil or the like, it is preferably a vacuum package or a shrink package from the viewpoint of ease of the coating step. In the case where the outer material is a ceramic coating, a resin coating or the like, it may be coated on the core material by means of a brush or a sprayer, and the material may be coated with the core material. Further, a linear depressed portion may be provided in the heat-insulating material including the core material and the outer material which is press-formed to impart softness to the heat-insulating material. The shape of the wire may be selected from a straight line, a curved line, a broken line or the like depending on the state of use of the heat-dissipating material, or two or more of these may be combined. The thickness of the line and the depth of the depressed portion can be determined according to the thickness, strength, and use condition of the heat-insulating material. The outer material can cover the entire surface of the core material, and can also partially cover the core material. [4] Use of the powder-like heat-insulating material containing the cerium oxide particles and/or the oxidized granules of the present embodiment, the formed heat-dissipating material, and the heat-insulating material having the outer material, in addition to the heat-dissipating material In addition, it can also be preferably used for: sound absorbing material 1 · bucket tamper material, sound insulation material, echo prevention material, sound absorbing material, abrasive catalyst carrier, adsorbent, adsorbing fragrance or bactericide, etc. Deodorant, deodorant, humidity control material, filler, pigment f 0 [5] Determination of parameters by the following method, the thermal conductivity of the thermal insulation material, BET specific surface 158675.doc 51 201228989 product, fog The measurement of the packing bulk density, the measurement of the content rate of an alkali metal element, etc., the depth evaluation of the mold required for press molding, the measurement of the rebound, the measurement of the compressive strength, and the measurement of the cumulative pore volume. [Measurement of thermal conductivity] The center of the styrene resin foam having a length of 30 cm, a width of 30 cm, and a thickness of 5 cm was cut into squares of 24 cm in length and 24 cm in width to form a styrene resin bubble frame. A concave portion was formed as a sample stage by adhering an aluminum foil of 3 〇 crn and a width of 30 cm to one side of the frame. Further, the surface covered with the aluminum foil was used as the bottom surface of the sample stage, and the other surface in the thickness direction of the styrene resin foam was used as the top surface. The powdery heat-breaking material was not slammed or pressurized, and was filled in the concave portion. After scraping, an aluminum foil having a length of 30 cm and a width of 30 cm was placed on the top surface, and the obtained sample was used as a measurement sample. Using the measurement sample, the heat flow meter HFM 436 Lambda (trade name 'NETZSCH Co., Ltd.) was used to measure 3 (the thermal conductivity under TC ° calibration system was based on 118 8 1412-2, using density 163.12 1 &lt;^/1113, thickness 25.32 mm NIST SRM 1450c calibration standard plate, at a temperature difference of 2 ° ° C between the high temperature side and the low temperature side, at 15 ° C, 20 (:, 24 ° C, 30 ° C, 40 ° C ' 50 Calibration is performed in advance at °C, 60 °C, and 65 °C. In the case of measuring the heat-insulating material formed, it is formed into a molded body having a shape of 3 cm, 30 cm, and 20 mm. The thermal conductivity of the sample was measured according to the method of JIS A 1421-1, and a disk-shaped 2-piece thermal material having a diameter of 30 cm and a thickness of 20 mm was formed as a measurement sample. The measuring device was measured by a thermal plate method using a protective hot plate method (manufactured by Hidehiro Seiki Co., Ltd.) [Measurement of BET specific surface area of heat-dissipating material] 158675.doc

S 201228989 The specific surface area of the powder (nitrogen adsorption method) was measured by using a gas adsorption amount measuring device "Autosorb 3MP" (trade name) manufactured by Yuasa Ionics Co., Ltd. using nitrogen as an adsorption gas. The specific surface area is the BET method. [Determination of Loose Bulk Density of Powder] Loosely packed bulk density measuring device model MVD-86 manufactured by Tsutsui Ricoh Chemical Co., Ltd. 'Disperse the sample through a mesh of 500 μηι by means of electromagnetic vibration , drop and put into a sample container of 1 mL. After the completion of the filling of the sample, the sample was smoothed by a doctor blade, the weight was measured, and the density was calculated, and the obtained value was taken as a loose bulk density. In the case of a heat-insulating material containing inorganic fibers, inorganic fibers may remain on the screen. In this case, the components that have passed through the screen and dropped into the sample container are measured as described above, and are used as looseness of the heat-insulating material. Fill the bulk density. It is not limited to inorganic fibers. When any material remains on the net, the heat-insulating material that has fallen through the screen into the sample container is similarly loaded as a loose filling of the heat-dissipating material [the content of alkali metal elements, etc.) Measurement] The (four) heat-breaking material was pulverized using an agate mortar. It is really filled in a 30 譲 = PVC ring, and a small piece is used as a measurement sample by a dicing agent. When using the fluorescent X-ray analyzer RIX_3_ manufactured by the copy = limit 2 to measure the == formed heat-dissipating material, the metal element (4) U (4) can also be measured by (4).料 [Evaluation of the depth of the forming die required for press forming] 158675.doc -53- 201228989 It is assumed that the powder is filled into a forming die for press forming to produce a vertical length of 3 cm, a width of 30 cm, and a thickness of 20 In the case of a molded body having a bulk density of 〇5 g/cm3, the required amount of the raw material powder is 900 g. When a molded body having a bulk density of 1.0 g/cm3 is produced, the amount of the raw material powder is required. 18〇〇g When the loose bulk density of each carcass is less than 0.5 g/cm3', the powder volume at 900 g is calculated according to the loose bulk density, and the loose bulk density is 0.5 g/cm3 or more. At that time, the powder volume at the time of 18 〇 0 g was calculated from the loose bulk density, and the desired depth for obtaining the forming dies of the above-mentioned molded body was calculated. [Measurement of the rebound] The size of the inorganic mixture (the above-mentioned small particles and large particles, and if necessary, the entire mixed powder of infrared light-shielding particles or inorganic fibers) is fixed in the horizontal direction. In the state in which the inorganic mixture is applied in a vertical direction to obtain a molded body of a specific bulk density, the inorganic mixture is applied in a state in which the force is applied (four (4) is set to T丨 in the vertical direction, and after pressing, the The size of the molded body in the direction is maintained at a fixed height, and the thickness in the vertical direction of the molded body of the office is set to T2, and the ratio of the Τ2 phase to the T + f to the D1 is measured. The thickness increase rate of the molded body is 100×TVT丨[%]' by this - 疋仃-f mussel. Further, the "horizontal AJ system" is used, for example, to fill the square or cylinder as an inorganic mixture of the raw material of the shaped body. The state of the frame-shaped mold. [Measurement of Compressive Strength] The formed 埶 埶 钮 button is processed into a length of 2 cm, a width of 2 cm, and a thickness of 2 cm, using the Shimadzu Corporation's shares right, drought 2 Cm limited the company Made of precision universal test 158675.doc

S •54· 201228989

Autograph AG-100KN, the compression strength was measured at a pressing speed of 0.5 mm/min. [Measurement of cumulative micropore volume] Using the micropore distribution measuring device model AutoPore 9520 (manufactured by Shimadzu Corporation), the cumulative micropore volume was measured by a mercury infiltration method. The formed heat-dissipating material is cut into a growth cube so as to be inserted into a cell, and one to a low-sensitivity measuring unit is used, and the initial pressure is about 7 kPa (about 1 psia 'equivalent The pressure measurement was carried out under the conditions of a micropore diameter of about 180 μm. In the measurement, the mercury parameter is set to 130° for the mercury contact angle and 485 dyne s/cm for the mercury surface. [Examples] Hereinafter, the present invention will be described in more detail by way of examples, but the invention is not limited to the examples. The present invention can be implemented not only by the following embodiments, but also by various modifications, and the modifications are also included in the scope of the invention. Further, the measurement of the thermal conductivity in the examples and the comparative examples, the measurement of the looseness of the looseness of the powder, the evaluation of the depth of the molding die required for the press molding, and the measurement of the rebound were as described above. [Example 1] A cerium oxide powder (small particle) having an average particle diameter of 14 nm (a small particle) of 1% by mass and a cerium oxide powder (large particle) having an average particle diameter of 60 μm were supplied by a mass of 9 〇 by mass. The honing machine was uniformly mixed to obtain the powdery heat-insulating material of Example 1. The heat-insulating material has a BET specific surface area of 20 m 2 /g and a thermal conductivity of 0.0479 W/m at 30 ° C. The loose packing density of the heat-insulating material is 〇 62 g/cm 3 , and accordingly, the volume of the heat-dissipating material 18 〇〇 g of Example 1 is 158675.doc • 55- 201228989 , / 〇 · 62 - 2903 cm. Therefore, it is assumed that the inner stern is used in the case of using a heat-dissipating material of the embodiment ι to produce a molded body having a length of 30 cm, a width of 30 cm, a thickness of 2 〇, and a bulk density of 1 〇. The depth required for the forming die with a P dimension of 3〇em and 3〇em is (10)...(4)(4)”^Additional use of 1638 g of heat-dissipating material for your use, with internal dimensions of 30 cm in length and 30 in width The mold of cm is pressed and formed into a heat-dissipating material of longitudinal 3〇 (10), horizontal (10), and thick 2, and a bulk density of 〇·91 ～3. The thickness increase rate at this time is 1G3%. When the powder-like heat-dissipating material of Example i is injected into the hopper, the powder is scattered or agglomerated less, and the filling into the forming mold is smooth. The same method is used to produce a heat-dissipating material formed by forming a sheet. The delamination was suppressed in any of the forming bodies, and no forming defects were observed. In addition, the thermal conductivity at 30 eC of the formed heat-insulating material was 〇〇478 w/m·κ. [Example 2] 25% by mass of 2.7 nm of SiO 2 powder (small particles) and a dioxide powder with an average particle size of 6 _ (large particles are still mass% mixed by a chain mill, The powder-like breaking material of Example 2 was obtained. The briquette specific surface area of the heat-dissipating material was 91 m2/g, and the guiding rate of the third generation was WKe. The loose bulk density of the material was 0.075 g/em. Accordingly, the volume of the heat-dissipating material of Example 2 of 900 g was calculated in the same manner as in Example (4), and the result was 12 〇〇〇ο〆. Therefore, 俨# When the heat-dissipating material of the actual course is used to manufacture a heat-dissipating material having a length of 3 cm and a thickness of '2 mm thick and a looseness of 〇.5 g/cm 3 is calculated in the same manner as the embodiment! The depth required for the forming die is 13 - 3 cm. In addition, the heat-dissipating material 936 of the embodiment 2 is used and the actual I58675.doc _56_

S 201228989 The same mold as in Example 1 was subjected to pressure forming to obtain a formed heat-dissipating material having a length of 30 cm, a width of 30 mm and a thickness of 2 mm, and a bulk density of 〇52 g/cm3; the thickness increase rate of the plucked was 1 〇. 60/〇. When the powdery heat-insulating material of Example 2 was charged into the hopper, the powder was scattered or aggregated less, and the filling into the forming crucible was also smooth. By the same method, the 1() piece is formed by the forming, and the material is layered in the &lt;壬&amp; shape to be suppressed, and no shape is formed, and the heat of the star-shaped heat-dissipating material at 30 ° C is obtained. The conductivity is 0.0301 W/m · K 〇 [Example 3] The average particle diameter of 14 nm and the average particle diameter of 1 〇μιη of di-dicarbide powder (small particles) 25% by mass, cerium oxide powder The body (large particle) of 75 mass% was uniformly mixed by a hammer mill to obtain the powdery heat-insulating material of Example 3. The BET specific surface area of the heat-sensitive material is 49 m2/g, and the thermal conductivity of 3()tT is °·0313 W/m · K. The loose packing density of the heat-insulating material was 〇. 〇ί 细3, and accordingly, the volume of the heat _g was calculated in the same manner as in Example i, and the result was 9 cm 3 . Therefore, it is assumed that the heat-dissipating material of the third embodiment is used to produce a vertical length of 3 〇 cm, a horizontal width, and a thickness of 2 〇 ,, and (4) when the degree is a molded body, the depth required for the forming mold is calculated by the same formula as the embodiment. The result is u〇cm. Further, the heat-dissipating material of the third embodiment is the same as that of the first embodiment, and the forming material 3 is obtained by forming a heat-dissipating material having a length of 30 cm, a width of 3 〇 (10), a thickness of 2 〇, and a bulk density of (10). The thickness increase rate at this time is chat. When the powdery heat-insulating material of Example 3 was charged into the hopper, the scattering or agglomeration of the body was small, and the filling into the forming mold was smooth. Lee: 158675.doc •57* 201228989 Manufactured by the same method] The heat-dissipating material of the enamel sheet was formed by delamination in any of the formed heat-dissipating materials, and no forming defects were observed. In addition, the thermal conductivity at 30 t of the thin-form heat-breaking material is 〇〇3i4w/m.K. [Example 4] The average particle was given as 14 (10): oxygen-cut powder (small particle weight %, and di-oxy-cut powder having an average particle diameter of 5 G nm (large particle Gulf% by the clock mill Sentence mixing 'to obtain the powdery (four) material of Example 4. The (4) specific surface area of the heat-insulating material is as follows: guide = ° ° ° 2993 · K. The loose bulk density of the heat-insulating material is (4) :: According to this, in the same manner as in Example 1, the body heat of 900 g of the heat-insulating material of Example 4 was calculated, and the volume result of ^士/1〇/^ g疋 was 13〇43 cm3. In the case where the heat-dissipating material of the second example 4 is made of a longitudinal heat-dissipating material of 3 〇 (10), 30 cm horizontally, and 20 rif two g/em3t_ shape, the depth required for the forming die is calculated in the same manner as the result. 5 coffee. In addition, using the heat-dissipating material of Example 4, 9Mg, using the factory mold to press and press form 'to obtain a length of 30 cm, a width of 30 cm, a thickness of 20 mm, and a bulk density of 〇53 §/post material. The thickness increase rate of the time is _. When the hot material is broken into the material in the hopper, the scattering or agglomeration of the powder is smoother than that of the embodiment 4. The method of making ^ 乂 成形 成形 成形 成形 任一 任一 任一 任一 任一 Λ Λ Λ Λ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ μ The thermal conductivity of the thermal material under the armpit.._ [Example 5] 158675.doc

S -58- 201228989 35 mass% of cerium oxide powder (small particles) having an average particle diameter of 14 nm, and cerium oxide powder (large particles) having an average particle diameter of 320 nm, 65 masses by hammer grinding The machine was uniformly mixed to obtain the powdery heat-breaking material of Example 5. The heat-insulating material had a BET specific surface area of 74 m2/g and a thermal conductivity of 0.0293 W/m·K at 3 〇t. Loose filling of the thermal insulation material. ·. - According to this, the volume of the heat-dissipating material 900 g of the actual = was calculated in the same manner as in Example ,, and as a result, it was 24684 cm3. Therefore, assuming that a heat-dissipating material of Example 5 is used to produce a shaped heat-insulating material having a length of 3 〇 cm, a width of 3 〇 cm 'thick mm, and a bulk density of 0 J g/cm 3 , the same as in the first embodiment. The depth required for the forming die was calculated and found to be 26.3 cm. Further, using the heat-dissipating material 6 of Example 5, press molding was carried out by the same mold as in Example 1, and a longitudinal 3 〇 cm, a width of 3 〇 (10), and a thickness of 20 mm were obtained, and the bulk density was 〇·47 g/ The formed heat-dissipating material of cm3. The thickness increase rate at this time was 106%. When the heat-breaking material of Example 5 was charged into the hopper, the powder was scattered or agglomerated less, and the filling into the forming mold was also smooth. One piece of the formed heat-dissipating material was produced in the same manner, and as a result, delamination was observed in one of the sheets, and the remaining 9 sheets were layered to be suppressed, and no forming defects were observed. In addition, the thermal conductivity of the formed heat-insulating material was 0.0294 W/m·K. [Example 6] 4% by mass of cerium oxide powder (small particles) having an average particle diameter of 12 nm and 60% by mass of cerium oxide powder (large particles) having an average particle diameter of 100 M·111 The key mill was mixed uniformly to obtain the powdery heat-breaking material of Example 6. The thermal insulation material has a BET specific surface area of 91 m2/g, and 3 (the thermal conductivity of 158675.doc -59 - 201228989 is 469 y / W · m · K. The loose bulk density of the thermal insulation material is 184 g According to this, the volume of the heat-dissipating material 9 〇〇g of the embodiment 6 is 4891 cm, and it is assumed that the longitudinal (10), the transverse 3 〇 (10) 'thickness 20 _, the bulk density is produced using the heat-breaking material of the embodiment 6. In the case of a 0.5 g/cm3 shaped heat-dissipating material, the depth required for the forming mold was calculated to be 54 cm in the same manner as in the example. In addition, the heat-dissipating material 1044 g of Example 6 was used, Press forming was carried out by the same mold as in Example 1 to obtain a formed heat-dissipating material of longitudinal 30 em, transverse 3 G em, thickness 2 Q _, and bulk density of (iv) _ 3. The thickness increase rate at this time was _" into the hopper. When the heat-insulating material of the embodiment 6 is put into use, the powder is scattered or agglomerated less, and the filling to the forming mold t is also smooth. By the same method (4) the iq sheet is formed into a broken (four) material, and the heat is broken. The delamination of the material towel is suppressed. 'No formation defects are found. ^In addition, the thermal conductivity under the machine of the formed heat-dissipating material is 0.046. 8 W/m · K. [Example 7] A cerium oxide powder (small particle) having an average particle diameter of 14 nm (three particles) and a cerium oxide powder having an average particle diameter of 80 nm (large particles) 7 〇 mass% was uniformly mixed by a hammer mill to obtain a powdery heat-dissipating material of Example 7. The BET specific surface area of the heat-insulating material was 82 m 2 /g, and the thermal conductivity at 3 〇 t It is 0.0237 W/m·K. The bulk density of the heat-dissipating material is g/cm3'. According to this, the volume of the heat-dissipating material 9〇〇g of the embodiment 7 is 丨^^ cm3. Therefore, it is assumed that the embodiment is used. When the heat-dissipating material of 7 is used to produce a molded body having a vertical length of 30 cm and a thickness of 20 mm and a bulk density of 〇.5 g/cm 3 , the depth required for the forming mold is calculated in the same manner as in the first embodiment. 158675.doc -60· 201228989 The fruit was 15.4 cm. In addition, the heat-insulating material 75 of Example 7 was used, and the same mold as in Example 1 was used for press forming to obtain (4) (10), horizontal ^ cm, and thickness 20 _ 'The cut-off density is 42.42 g/cm3 of the formed heat-dissipating material. The thickness increase rate at this time is Cong. When the heat-insulating material of Example 7 is put into the hopper, the powder is scattered. The agglutination was less, and the filling into the forming mold was smooth. The heat-dissipating material formed by forming the one-piece sheet was obtained by the same method, and the heat-dissipating material of the heat-dissipating material of the (4) was obtained by (4), and no forming defects were observed. In addition, the thermal conductivity at 3 〇t of the formed heat-dissipating material is 〇〇236 W/m · K 〇 [Example 8] Silica sand powder (small particles) having an average particle diameter of 14 im 2 % of 〇f, and alumina powder (large particle) having an average particle diameter of 200 nm, 8 〇 mass% are uniformly mixed by a honing machine', and the powdery heat-dissipating material of Example 8 is obtained. The thermal material has a specific surface area of 45 m2/g, and the thermal conductivity of the grab is 丨) fine W/m·K. The bulk density of the heat-insulating material is (4) 5 fine 3, palpitations, and the volume of the heat-breaking material _ g of the embodiment 8 is _8 (10) 3. Therefore, it is assumed that the case of using a heat-dissipating material of Example 8 to produce a longitudinally-cut coffin having a longitudinal density of 2 mm, a thickness of 2 mm, and a bulk density of 〇5 g/cm3 is used in the embodiment. The depth required for the calculation of the forming die was calculated to be 11_8 cm. In addition, the heat-dissipating material of Example 8 was used, and the same mold as in Example 1 was used for press forming to obtain a longitudinal Mm and a horizontal 3 Cm. The thickness is 20, and the bulk density is 72.72g/cm3 of the formed heat-dissipating material. The thickness increase rate at this time is secret. When the powder of the eighth embodiment is cast into the hopper, the powder is scattered or agglomerated. The filling in the mold is smooth, and the forming of the 1G sheet is formed by the same method. The material is delaminated in any of the formed bodies, and no forming defects are observed. The heat conductivity at 30 ° C of the formed heat-dissipating material was 0.0271 W/m · K. [Example 9] 15 mass% of alumina powder (small particles) having an average particle diameter of 7 nm, and The average particle L is 80 nm of the dioxide dioxide powder (large particles) 85 mass% is uniformly mixed by the honing machine to obtain the implementation. The powdery heat-breaking material of Example 9. The BET specific surface area of the heat-insulating material is 62 m2/g, 3 〇····κ. The loose bulk density of the powder = g/(10), according to which The volume of the heat-dissipating material _g of Example 9 is (10) 3. Therefore, it is assumed that the heat-dissipating material of Example 8 is used to manufacture the formed material of the longitudinal (10), (four) (10), and thick 20-faced bulk density of 〇.5 gW. In the case of the case, the second degree required for the molding die was calculated in the same manner as in Example 14 and the result was 8.85 cm. Further, the same mold as in Example 1 was used using the heat-insulating material g' of Example 9. Adding M to form a heat-dissipating material of 3〇cm^, 3〇cm.#2〇mm,#^^〇54gW^^. The thickness increase rate at this time is 1〇6%. π in the hopper / Example 9 When the material is broken, the powder is scattered or agglomerated less, and the filling in the mold is smooth. The same method is used to make a sheet of crucible, and the material is broken into heat, and the heat is broken in the forming-forming. There is no forming defect in the material, and the formed heat-dissipating material has a P-system of 0.0262 W/m·K. [Example 10] 158675.doc - 62- 201228989 The cerium oxide powder (small particles) having an average particle diameter of 14 nm is 21 mass%/〇, and the cerium oxide powder (large particles) having an average particle diameter of 150 nm is 63% by mass. After the mixture was mixed, 16% by mass of ruthenium acid as an infrared light-shielding particle having an average particle diameter of 丨μηη was added, and the mixture was uniformly mixed to obtain a powdery heat-insulating material of Example 10. In the powder of Example 10. The ratio RL of the mass of the large particle to the mass of the small particle and the mass of the large particle is 75%. Further, the content of the lining acid was 0.21% by volume based on the total volume of the heat-insulating material. The thermal insulation material has a BET specific surface area of 52 m /g and a thermal conductivity of 302.7 C at 30 C. The unloaded bulk density of the thermal insulation material was 〇.〇61 g/cm3, and accordingly, the volume of the heat-dissipating material of Example 1 was 900 754 cm3. Therefore, assuming that the heat-dissipating material of the embodiment (7) is used to produce a shaped heat-dissipating material having a length of 30 cm, a width of 30 cm, a thickness of 2 〇, and a bulk density of ο" g/cm, The depth required for the forming die was calculated in the same manner and found to be 16.4 cm. Further, using the heat-dissipating material of Example 10, 1 〇 44 g, using the same mold as the embodiment: performing dusting forming 'to obtain 3 〇 cm in length, 3 〇 (10) in width, 2 〇 in thickness, and a bulk density of 0.58 g / The formed heat-dissipating material of cm3. The thickness increase at this time is ::102%. When the powder of Example 1 was put into the hopper, the powder was less likely to fly or aggregate, and the filling into the forming mold was smooth. The same t was used to make 1G&gt;|formed heat-dissipating material, which was layered in any of the formed bodies: to suppress 'no formation defects. In addition, the formed heat-dissipating material: 热c has a thermal conductivity of 〇 0275 w/m · κ. The second outer part uses 819 g of the powder-shaped heat-dissipating material separately, and press-forms it with a cylindrical mold of inner diameter ', 彳2 〇Cm, and obtains two pieces of straight _ 3〇158675.doc -63 - 201228989 Using the heat-dissipating material of the shape of the disk-shaped shaped heat-dissipating material sheet of the thickness (20) and the thickness of 20, the heat of 0.0 W 『c is 0.0851 W/m · K 〇

[Example 11J 2 〇 mass% of a rare earth oxide powder (small particle) having an average particle diameter of 14 nm and a mass of 6 〇 of a dioxide powder (large particle) having an average particle diameter of 150 nm. ^ After mixing with the grinders, add an average particle size of ι (4) as the infrared pre-particles, and then add 15 mass% of the particles, continue to mix and mix, and then add the average fiber diameter of ii μηι, average fiber. The powder-like heat-insulating material of Example 11 was obtained by mixing and homogenizing the glass fiber having a temperature of 5% by weight and using a high-speed shear mixer. In the heat-insulating material of Example 11, the mass of the large particles was 75% with respect to the total mass of the mass of the small particles and the mass of the particles. Further, the content of the sulphuric acid was 〇19% by volume based on the entire volume of the heat-insulating material. The heat-insulating material has a BET specific surface area of 5 〇 mVg and a thermal conductivity of 3 〇 ec at a temperature of W/m*K. The heat-insulating material has a packing density of 0.059 gW. According to this, the volume of the heat-insulating material _g of the example u is (10) c^m3. Therefore, it is assumed that the longitudinal % is produced using the heat-insulating material of Example u. In the case of a claw, a cross-section of 30 cm, a thickness of 20 mm, and a shape of a heat-insulating material having a bulk density of 〇·5 g/cm3, the depth required to calculate the forming mold in the same manner as in Example 1 was 16.9 cm. . Further, using the heat-dissipating material 7〇2 g of Example u, press forming was carried out by using the same mold as in Example ,, and a longitudinal 3 0 cm, a horizontal 30 cm, and a thick 2 bribe were obtained, and the bulk density was 〇% g/ The formed heat-dissipating material of cm3. The thickness increase rate at this time was 1〇2%. Into the hopper 158675.doc

S •64· 201228989 In the case of the heat-dissipating material of Example u, the scattering or agglomeration of the powder is smoother than the filling of the mold. The same method is used to make the heart (4) 2 heat-dissipating materials department's - the formed heat-dissipating material is obtained by layering, and the forming defects are seen. Further, the rate of the formed heat-insulating material was 0.0278 W/m·K. In addition, 551 g of the powder-shaped heat-dissipating material was separately used, and a cylindrical mold having a diameter of 30 cm was used for press forming, and two disk-shaped formings having a diameter of two cm and a thickness of 20 were obtained. Thermal insulation material. The thermal conductivity at 8 〇〇t was measured using the two formed heat-insulating materials, and the result was 0.0921 W/m*K. [Example 12] cerium oxide powder (small particles) having an average particle diameter of 7.5 nm] 9% by mass and 57% by mass of cerium oxide powder (large particles) having an average particle diameter of 80 0111 After uniformly mixing the hammer mill, 14% by mass of bismuth acid as an infrared light-shielding particle having an average particle diameter of 丨pm was added, and the mixture was uniformly mixed, and the average fiber diameter was 丨丨μιη, and the average fiber length was 64 mm. The heat-resistant temperature was 105 (10% by mass of the glass fiber of TC, and it was made uniform by mixing using a high-speed shear mixer, and the powdery heat-insulating material of Example 12 was obtained. In the heat-dissipating material of Example 12, large The mass of the particles is 75% relative to the total mass of the small particles and the mass of the large particles. Further, the content of the bismuth acid is 〇25 by volume based on the volume of the entire heat-dissipating material. The specific surface area is 89 m2/g, 30. (: the thermal conductivity is 0.0273 W/m · K. The loose bulk density of the heat-insulating material is ι8ι g/cm3 'According to this' embodiment 12 The volume of the heat-dissipating material 9〇〇g is 11U1 158675.doc -65- 201228989 cm Therefore, it is assumed that when the heat-dissipating material of Example 12 is used to manufacture a longitudinally-shaped jaw, a cross-section of 30 cm, a thickness of 20 mm, and a bulk density of 〇5 g/cm3, the shape of the heat-dissipating material is The depth required for the molding die was calculated in the same manner as in Example i, and was 12.3 cm. Further, using the heat-insulating material 972 g of Example 12, press molding was carried out using the same mold as in Example i to obtain a vertical 30-plus. The transverse 30-heart, thick 20 „1111, the bulk density is 经54 叭1113 formed heat-dissipating material. The thickness increase rate at this time is 1〇3%. When the powder of Example 丨2 is put into the hopper, the powder The body is scattered or agglomerated less, and the filling into the forming mold is smooth. The 1G sheet is formed into the heat-dissipating material by the same method, and the layered in any formed heat-dissipating material is restrained to prevent formation defects. In addition, 3 〇 of the formed heat-dissipating material. The thermal conductivity of the underarm is 0.0272 W/m · K 〇 In addition, the powder-shaped heat-breaking material 763 g is used, and the inner _ is 30 mm in diameter. The cylindrical mold is press-formed to obtain two discs with a diameter of (10) and a thickness of 2G. The formed heat-dissipating material. Using the two heat-insulating materials formed, 80 (the thermal conductivity of rCT is 1 0.131 W/m · K. ° is [Example 13] The average particle diameter is M nm The volume of the dioxide dioxide powder (small particles) is '%' and the average particle size is 6 _ dioxotomy powder (large particles) 51 mass. 由 borrowed by the grinder, the average is added The particle size of i μιη is 21% by mass of the red shading particles, and continues to be uniformly mixed. The average fiber diameter is η, the average fiber length is 64, and the heat resistance = glass fiber lf$%. High speed shear mixer mixing 158675.doc

• 66 - 201228989 and made uniform. The powdery heat-insulating material of Example 13 was obtained. In the heat-insulating material of Example 13, the ratio Rl of the mass of the large particles to the total mass of the small particles and the mass of the large particles was 65%. Further, the content of zirconium silicate is 〇5% by volume based on the entire volume of the heat-insulating material. The heat-breaking material has a BET specific surface area of 53 m2/g, 30. (The thermal conductivity underneath is 0.0288 W/m · K. The loose bulk density of the heat-insulating material is 0.110 g/cm 3 , and according to this, the volume of the heat-dissipating material of Example 13 is 8182 cm 3 . Assuming that a heat-dissipating material of Example 13 is used to produce a shaped heat-dissipating material body having a length of 3 〇cm, a width of 30 cm, a thickness of 20 mm, and a bulk density of 〇5 g/cm3, the same as in the embodiment. The depth required for the molding die was calculated and found to be 9.09 cm. Further, using the heat-dissipating material 1242 g of Example 13, press molding was carried out using the same mold as in Example , to obtain a length of 30 cm, a width of 30 cm, and a thickness of 30 cm. 20 mm, formed heat-insulating material with a bulk density of 0.69 g/cm3 "The thickness increase rate at this time is 丨〇3%. When the powder of Example 13 is put into the hopper, the powder is scattered or agglomerated less. And the filling into the forming mold is also smooth. The heat-dissipating material formed by forming the one-piece sheet by the same method is suppressed by layering in any of the formed heat-insulating materials, and no forming defects are observed. The thermal conductivity of the heat-dissipating material at 3〇〇c is 0.0289 W/m · K. Using the 975 g of the powder-shaped heat-breaking material, a cylindrical mold having a diameter of 30 cm was used for press forming, and two circular-shaped formed heat-insulating materials of a straight scale cm and a thickness of 20 mm were obtained. Using a sheet-formed heat-dissipating material, 80 (thermal conductivity at rc was measured and found to be 0.0480 W/m · K 〇 158675.doc • 67· 201228989 Table 1 shows the heat-insulating materials of Examples 1 to 13. Among them, Na, yttrium, Mg, Ca, Ge, P, and Fe are based on the total mass of the heat-insulating material. Table 2 shows the large particles contained in the heat-insulating materials of Examples 1 to 13. /

Na, K, Mg, Ca, Ge, P, and Fe are based on the total mass of the large particles. [Table 1] Content in the heat-insulating material Na [% by mass] K [% by mass] Mg [% by mass] Ca [% by mass] Ge [mass fjpm] P [% by mass] Fe [% by mass] Example 1 8.98 0.684 2.31 6.27 0 0.006 0.114 Example 2 0.074 1.06 0.005 0.020 0 0.003 0.081 Example 3 0 0 0 0 0 0.003 0.042 Example 4 0.274 0.712 0.430 0.161 0 0.168 0.740 Example 5 0.020 0.015 0.010 0.017 0 0.005 0.173 Example 6 5.99 0.477 1.54 4.30 0 0.003 0.089 Example 7 0 0 0 0 400 0 0.011 Example 8 0 0 0 0 0 0.001 0.002 Example 9 0 0 0 0 485 0.002 0.011 Example 10 0.218 0.561 0.339 0.140 0 0.023 0.596 Example 11 0.209 0.534 0.429 0.137 0 0.021 0.570 Example 12 0.004 0 0.213 0.020 325 0.019 0.025 Example 13 0.054 0.719 0.025 0.033 0 0.015 0.074 [Table 2] Content of the large particles in the example Na f mass % 1 K [% by mass % Mg " Mass %1 Ca f mass%1 Ge [mass ppm] P "mass%1 Fe" mass%1 Example 1 9.98 0.760 2.57 6.97 0 0.006 0.126 Example 2 0.098 1.41 0.007 0.027 0 0.003 0.106 Example 3 0 0 0 0 0 0.003 0.053 Example 4 0.342 0.890 0.538 0.201 0 0.020 0.923 Example 5 0.030 0.024 0.015 0.026 0 0.257 0.263 Example 6 9.99 0.795 2.56 7.16 0 0.006 0.14 Example 7 0 0 0 0 571 0.002 0.013 Example 8 0 0 0 0 0 0 0 Example 9 0 0 0 0 571 0.002 0.013 Example 10 0.342 0.890 0.538 0.201 0 0.020 0.923 Example 11 0.342 0.890 0.538 0.201 0 0.020 0.923 Example 12 0 0 0 0 571 0.002 0.013 Example 13 0.098 1.41 0.007 0.027 0 0.003 0.106 158675.doc -68 - 201228989 [Example 14] The formed heat-insulating material obtained in Example 3 was subjected to heat treatment at 1 Torr for 10 hours to obtain the heat-insulating material of Example 14. The heat-clear material was cut into 2 cm in length, 2 cm in width, and 2 cm in thickness, and the compressive strength was measured. The maximum load at a compression ratio of 5.0% was 081 MPa. Further, in the molded body of the heat-insulating material of Example 14, the ratio r of v to v〇 〇〇3 was 77.9%, and ν〇·()5 was 1.199 mL/g. [Example 15] The molded heat-insulating material obtained in Example 4 was subjected to heat treatment at 900 ° C for 5 hours to obtain a heat-insulating material of Example 15. The heat-insulating material was measured for compressive strength in the same manner as in Example 14. As a result, the sample collapsed at a compression ratio of -3.9% and showed a breaking point, at which time the load was 3 89 MPa. Further, in the molded body of the heat-dissipating material of Example 5, the ratio R of v to V0.003 was 98.2%, and V0.05 was 0.857 mL/g 〇 [Example 16] The obtained in Example 5 The formed heat-insulating material was heat-treated at 9 Torr for 1 hour to obtain the heat-insulating material of Example 16. The compressive strength was measured in the same manner as in Example 14 for the heat-insulating material, and the compression ratio = 4.7% of the sample collapsed and showed a breaking point, and the load at this time was 1〇9〇MPa. In addition, in the molded body of the heat-insulating material of Example 16, the ratio R of v to V0.〇〇3 was 81.5%. ▽0.05 was 1.109 mL/g [Example 17] The formed heat-insulating material obtained in Example 6 was subjected to heat treatment at 9 °»c for 2 hours to obtain a heat-insulating material of Example 17. Heat-dissipating material 158675.doc -69- 201228989 The compressive strength was measured in the same manner as in Example 14, and as a result, the sample collapsed at a compression ratio = 4.9% and showed a breaking point at which the load was 6.29 MPa. Further, Example 17 In the molded body of the heat-breaking material, the ratio R of V to V〇.o〇3 is 32.9%, and V〇.〇5 is 0.581 mL/g. [Example 18] The formed heat-insulating material obtained in Example 7 was subjected to heat treatment at 1 ° C for 5 hours to obtain a heat-insulating material of Example 18. The heat-insulating material was used and implemented. The compressive strength was measured in the same manner as in Example 14. As a result, the maximum load at a compression ratio of -5.0% was 〇·87 MPa. Further, in the molded body of the heat-insulating material of Example 16, the ratio of V to ν0.0〇3 R was 52.8%, and V〇.05 was 1.361 mL/g. [Example 19] The formed heat-insulating material obtained in Example 8 was subjected to heat treatment at 丨丨〇〇&lt;»c for $hour to obtain The heat-insulating material of Example 19. The compressive strength was measured in the same manner as in Example 14 for the heat-insulating material, and as a result, the sample collapsed at a compression ratio = 4.3% and showed a breaking point, at which time the load was ι.ΐ2 MPa. Further, in the molded body of the heat-insulating material of Example 19, the ratio R of v to V〇.〇〇3 was 87_6% 'V〇.〇5 was 1.097 mL/g. [Example 20] Example 9 The formed heat-dissipating material obtained in the obtained heat-treating material of Example 20 was obtained by performing a heat treatment for 5 hours under rc. The heat-dissipating material of Example 20. The compressive strength was measured in the same manner as in Example 14, and as a result, the sample collapsed at a compression ratio = 4.1% and showed a breaking point at which the load was 2 η MPa. Further, the formation of the heat-insulating material of Example 2 In the body, v is relative to 158675.doc •70- 201228989 V〇.o〇3 ratio R is 90.0%, Vow is 〇, 937 mL/g. [Example 21] The molded heat-insulating material obtained in Example 10 was subjected to heat treatment at 9 ° C for 5 hours to obtain a heat-insulating material of Example 21. The compressive strength was measured in the same manner as in Example 14 for the heat-insulating material, and as a result, the sample collapsed at a compression ratio = 4.5% and showed a breaking point, at which time the load was 3 MPa. Further, the heat-breaking material of Example 21 was formed. In the body, the ratio of v to V〇.o〇3 is 89.3%, and V〇.〇5 is 1.142 mL/g. [Example 22] The molded heat-insulating material obtained in Example 11 was subjected to heat treatment at 9 ° C for 5 hours to obtain a heat-insulating material of Example 22. The heat-insulating material was measured for compressive strength in the same manner as in Example 14. As a result, the sample collapsed at a compression ratio of -4.4% and showed a breaking point, at which time the load was 〇·% MPa. Further, in the molded body of the heat-insulating material of Example 22, the ratio R of v to V0.003 was 76.9%, %. 5 is i 〇 31 mL/g. [Example 23] The formed heat-insulating material obtained in Example 12 was subjected to heat treatment under the crucible for 24 hours to obtain the heat-insulating material of Example 23. The compressive strength was measured in the same manner as in Example 14 for the heat-dissipating material. As a result, the sample collapsed at a compression ratio of 3.4% and showed a breaking point, and the load at this time was 192 MPa. Further, in the molded body of the heat-insulating material of Example 22, the scale of v with respect to V0.003 was ..."%, and ¥5 was 1〇771^/§. [Example 24] The formed heat-insulating material obtained in Example 13 was subjected to heat treatment at 158 675.doc • 71 - 201228989 at 9 Torr (&gt;c, to obtain the heat-insulating material of Example 24. The heat-insulating material was measured for compressive strength in the same manner as in Example 14. As a result, the maximum load at a compression ratio = 5.0% was 0.75 MPa. Further, in the molded body of the heat-insulating material of Example 24, 'V vs. V0. The ratio r of 〇3 was 48.1%, and v〇〇5 was 0.691 mL/g. [Comparative Example 1] The cerium oxide powder 丨 00% by mass of an average particle diameter of 14 nm was used as the powder of Comparative Example 1. The thermal insulation material has a bet specific surface area of 195 m2/g, and a thermal conductivity of 3 〇·〇ΐ 8 w/m · κ at 3 ° C. The loose bulk density of the thermal insulation material is 〇. 〇1〇7 g/cm3, according to this comparative example, the volume of the heat-dissipating material 900 g is 84112 cm3. Therefore, it is assumed that the heat-dissipating material of Comparative Example 1 is used to make a longitudinal 30 cm, a horizontal 30 cm, a thickness of 2 mm, and a pine. In the case of a shaped heat-dissipating material having a density of 〇5 g/cm3, the depth required for the forming mold was calculated in the same manner as in Example}, and the result was 93.5 cm. Further, using 3 〇 6 g of the heat-insulating material of Comparative Example 1, press molding was carried out by the same mold as in Example 1, and a longitudinal 〇 3 cm, a width of 3 〇 cm, and a thickness of 2 〇 claws were obtained, and the bulk density was 〇· 17 g/cm3 of the formed heat-insulating material. The thickness increase rate at this time was 132%. When the heat-damping material of Comparative Example 1 was put into the hopper, the powder was significantly scattered and agglomerated on the supply line, which was difficult to uniformly fill. In the forming mold, the same method is used to produce a heat-dissipating material formed by menstruation. As a result, the forming defects are generated in the formed heat-insulating material. Therefore, the thermal conductivity at 30 eC of the formed heat-insulating material cannot be measured. [Comparative Example 2] The average particle diameter was 1 〇μηΐ2 cerium oxide powder 1 〇〇 mass. 'As a comparison 158675.doc

S • 72· 201228989 Example 2 &amp; The thermal insulation material has a bet specific surface area of 〇·27 m/g and a thermal conductivity of 30 636 w/m·κ at 30C. The bulk density of the heat-dissipating material was 〇.693 g/cm3, and the volume of the heat-dissipating material of Comparative Example 2 was 1800 g, which was 2597 cm3. Therefore, it is assumed that the heat of the comparative example is used to produce a shaped heat-dissipating material having a length of 30 cm, a width of 30 cm, a thickness of 2 mm, and a bulk density of 〇5 g/cm. The depth required for the forming die was calculated in the same manner and found to be 2.89 Cm. Further, using 1458 g of the heat-insulating material of Comparative Example 2, press molding was carried out by the same mold as in Example 1, and a warp shape of 30 cm in length, 30 cm in width, 2 mm in thickness, and a bulk density of 0.81 g/cm3 was obtained. The material of the heat-breaking material. The thickness increase rate at this time was 108%. When the powder of Comparative Example 2 was charged into the hopper, the powder was less scattered, but aggregated on the supply line, and it was difficult to uniformly fill the molding die. Ten pieces of the formed heat-insulating material were produced by the same method, and as a result, any of the formed heat-insulating materials was brittle and collapsed when taken out from the mold. Therefore, it is impossible to measure the 3〇 of the formed heat-insulating material. (The thermal conductivity of the lower layer. [Comparative Example 3] A cerium oxide powder (small particle) having an average particle diameter of 14 nm, 8 Å mass 0 / 〇, and a cerium oxide powder having an average particle diameter of 60 μηι (large particle) 2% by mass was uniformly mixed by a hammer mill to obtain a powdery heat-insulating material of Comparative Example 3. The BET specific surface area of the heat-insulating material was 158 m 2 /g, and the heat at 3 〇t The conductivity is 0.0212 W/m · K. The loose bulk density of the powder is 〇〇126 g/em3'. The volume of the powder of Comparative Example 3 900 g is 71429 cm3. Therefore, it is assumed that Comparative Example 3 is used. The heat-dissipating material is manufactured in the same manner as in the first embodiment in the case of a formed heat-dissipating material of 30 cm in length, 3 cm in width, 20 mm in thickness and 0.5 g/cm 3 in bulk density. 158675.doc -73-201228989 The depth required for the calculation of the forming die was 7 9.4 c iti. In addition, the heat insulating material of Comparative Example 3 was used, and the same mold as in Example 1 was used for pressurization &amp; Longitudinal 30 horizontal 30cm, thick 20mm 'loose density is 〇27g/cm3 of formed heat-insulating material. The thickness increase rate at this time is recognized. In the case of the heat-dissipating material of Example 3, the powder was significantly scattered and agglomerated on the supply line. It was difficult to uniformly fill the forming mold. The same method was used to produce a heat-dissipating material which was formed into a sheet. The forming defects were generated in the heat-insulating material. Therefore, the molded article 30 could not be measured. (The following thermal conductivity. [Comparative Example 4] The formed heat-insulating material obtained in Comparative Example 1 was 9 〇 (rc The heat treatment was carried out for the next hour to obtain the heat-insulating material of Comparative Example 4. The compressive strength was measured in the same manner as in Example 14 for the heat-insulating material, and as a result, the maximum load at a compression ratio of 5.9% was 0.11 MiPa. Comparative Example 5] 1368 g of cerium oxide powder having an average particle diameter of 15 Å was used, and press molding was carried out in the same manner as in Example 1 to obtain a molded body, followed by heating treatment for 5 hours under a kiln technique. The heat-insulating material of Comparative Example 2 was obtained. The compressive strength was measured in the same manner as in Example 14 for the heat-insulating material, and as a result, the maximum load at a compression ratio = 5.0% was 0.17 MPa, and the thermal conductivity at 30 °C. 0.119 W/m · K 〇 [industrial availability j root Scattering the present invention 'provides a shaped or filled when the time obtained suppressed I58675.doc

S • 74-201228989 Excellent in manufacturability The production of a heat-insulating material with good moldability and a method for producing the same. Further, the present invention can provide a heat-insulating material formed by using a powdery heat-insulating material, and a heat-insulating material covering body containing a material other than the heat-insulating material. BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a view showing the relationship between the bulk density of loose bulk and the content rate rl of large particles. Fig. 2 is a photograph showing an example of a measuring device for loose bulk density. Fig. 3 is a schematic cross-sectional view showing a heat insulating material having an outer material according to an embodiment of the present invention. Fig. 4 is a schematic cross-sectional view showing small particles and large particles contained in the heat insulating material according to an embodiment of the present invention. [Main component symbol description] 1 Heat-dissipating material covering 2 Heat-dissipating material 3 External material L Large particle S Small particle 'I58675.doc

Claims (1)

201228989 VII. Patent application scope: .1. A powder-like heat-dissipating material containing a plurality of small particles including quartz dioxide and/or alumina and having a particle diameter Ds of 5 nm or more and 3 〇 nm or less. The BET specific surface area of the powdery powder of the particles is 5 m 2 /g or more and 150 m 2 /g or less, and the thermal conductivity at 3 〇 t is 0.05 w/m·K or less. The heat-insulating material of claim 1 has a loose bulk density of 0.030 g/cm3 or more and 0.35 g/cm3 or less. *5' such as the heat-breaking material of Kiss 1 which further contains a plurality of large particles including silica sand and/or alumina, having a particle size DL of 50 nm or more and 1 〇〇μπια, and the mass of the large particles The proportion of the mass of the small particles and the mass of the large particles is 60% by mass or more and 9% by mass or less. I. The heat-dissipating material of claim 2, which further comprises a plurality of large particles comprising cerium oxide and/or aluminum oxide having a particle size DL of 50 nm or more and 1 〇〇μηι&amp; and the mass of the large particles The ratio rl to the total of the mass of the small particles and the mass of the large particles is 6 〇 mass. /〇 above, below 9〇 quality. The heat-dissipating material of any one of claims 1 to 4, which contains infrared light-shielding particles, 800. (The thermal conductivity is 0.2 W/m · κ or less. 6. The heat-insulating material of claim 5, wherein the above-mentioned infrared light-shielding particles are flat. The average particle diameter is 〇·5叩 or more and 3〇μΓη or less. The volumetric content of the infrared ray-shielding particles is 〇2 vol% or more and 5% by volume or less based on the total volume of the heat-insulating material. 7. The heat-insulating material according to any one of claims 4 to 4, which contains At least one of the group consisting of a free alkali metal element, a soil-measuring metal element, and a faulty group, containing at least one element selected from the group consisting of the above-mentioned metal element and the soil-measuring metal element 158675.doc 201228989 In the case of the content of the heat-insulating material, the content is 5% by mass or more and 5% by mass or less based on the total mass of the heat-insulating material. When the cerium is contained, the content is based on the total mass of the heat-insulating material. The heat-insulating material of claim 7, wherein the at least one element selected from the group consisting of an alkali metal element, an alkaline earth metal element, and cerium is contained in the above-mentioned large In the particle. The heat-insulating material of any one of the above-mentioned items, wherein the content of the inorganic fibers is more than 0% by mass and not more than 2% by mass based on the total mass of the heat-insulating material. The heat-insulating material according to any one of claims 1 to 4, which contains phosphorus, and the phosphorus content is 0 to 002% by mass or more and 6 to 6% by mass or less based on the total mass of the heat-insulating material. The heat-insulating material according to any one of items 1 to 4, which contains iron and has a content of iron of 0.005 mass% or more and 6 mass% or less based on the total mass of the heat-insulating material. A thermal material obtained by forming a powdery heat-breaking material of any one of the claims 丨 to 13.. 13. The heat-insulating material of claim 12 has a compression ratio of 〇 5% The maximum load is 〇·7 MPa or more. 14. According to the heat-insulating material of Item 13, the cumulative pore volume V of the pores having a pore diameter of 0.05 μm or more and 0.5 μΐΏ or less is 0.003 μm or more with respect to the pore diameter of '1 50 Ratio of cumulative micropore volume ν〇〇〇3 of micropores below μιη r is 70 /. The above pore size is 〇〇5 or more, 15〇μηη below the micropores 158675.doc S -2- 201228989 Cumulative micropore volume v0.4〇.5mL/g or more, 2mL/^ 15. The heat-insulating material of any one of claims 1 to 4, 12 to 14 in the outer material material is contained in the heat-insulating material of claim 15 , wherein the above-mentioned outer material of Dan A contains Yi Jianmin. Or the above-mentioned outer material is a resin film. Fiber 17. A method for producing a heat-insulating material, comprising the steps of: containing cerium oxide and/or aluminum oxide, and having an average particle diameter of 5 nm or more and (10) or less Small particles, and large particles containing dioxo and/or oxidized, and having an average particle diameter of 50 nm or more and 100 (four) or less, in terms of the mass of the large particles relative to the mass of the small particles and the mass of the large particles 60 mass% or more and 90 mass% or less are mixed. 18. A method for producing a heat-insulating material, comprising the steps of: oxidizing a small particle comprising ceria and/or alumina and having an average particle diameter of 5 nm or more and 3 〇 1 claw or less; Shi Xi and/or Oxidation, and at least one element selected from the group consisting of alkali metal elements, alkaline earth metal elements and lanthanum, and having a large particle diameter of 50 nm or more and 1 〇〇μπι or less, The ratio of the mass of the large particles to the total mass of the small particles and the mass of the large particles is 60 mass ❹ /. The above mixture is mixed with 9 〇 mass% or less to obtain an inorganic mixture. A method for producing a heat-insulating material, comprising: arranging a small particle containing cerium oxide and/or aluminum oxide and having an average particle diameter of nm or more and 30 nm or less, and containing cerium oxide and/or oxidizing Aluminum, and at least one element selected from the group consisting of an alkali metal element, an alkaline earth metal element, and cerium, and having an average particle size of nm or more and 1 〇〇I58675.doc 201228989 μηι or less, as large particles The quality is relative to the mass of small particles. The ratio I of the total mass of the large particles is 60% by mass or more, 90% by mass, and the mixture is added to obtain an inorganic mixture; the accommodating step, the inorganic mixture is contained in the forming mold, and the forming step, The inorganic mixture is formed; and the forming step comprises the following step (4) or step (8): (4) heating the inorganic mixture to 40 Torr while pressurizing the inorganic mixture by the forming die. 〇 The above steps; () The step of subjecting the inorganic mixture to a pressure by pressurization, and then performing a heat treatment at a temperature higher than 艽. 20. The method of producing a heat-insulating material according to Item 19, wherein in the forming step, the bulk density of the heat-insulating material formed is 〇25 g/cm3 or more ' 2.〇g/cm3 or less The setting pressure is set. 21. A method of producing a thermal insulation material, comprising: comprising small particles having an average particle diameter of 5 nm or more and 30 nm or less, comprising ceria and/or oxidized, and comprising cerium oxide and/or oxidizing Ming, and at least i elements selected from the group consisting of metal elements, soil metal elements and faults, and having an average particle diameter of 5 〇 nm or more ' ι〇〇^ 乂 under the large particles, with large particles The ratio of the mass to the total mass of the small particles and the mass of the large particles RL is 60 mass % / 0 or more and 9 〇 mass 〇 / ❶ or less to obtain an inorganic mixture; Storing in the forming mold; forming step of forming the inorganic mixture; and cutting step, partially cutting the formed body obtained by the forming step; and the forming step 158675.doc 201228989 includes the following step (4) or Step (4): (4)-surface: pressurizing the inorganic mixture by the forming die so that the bulk density of the formed heat-insulating material is 〇25 W or more and 2.0 g/cm3 or less Heat step; (d) after pressurizing by using the molding die and the shaping of the inorganic mixture, a heat treatment step implemented at 40 (above the temperature TC 158675.doc.