JP2011219309A - Method for producing alumina particle with aln modified layer, and modified alumina powder - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a method for obtaining modified alumina particles by forming a modified layer comprising aluminum nitride (AlN) on at least part of a surface of alumina particles, and to provide modified alumina powder comprising modified alumina particles obtained by the method.SOLUTION: The method for producing alumina particles with an AlN modified layer includes kneading alumina powder comprising alumina particles whose particle diameter is ≥7 μm with a carbon dispersion liquid in which carbon is dispersed, and forming a modified layer comprising aluminum nitride on at least part of a surface of the alumina particles by a heat treatment by which the alumina powder with adhered carbon is kept at a temperature of 1,400-1,700°C for ≥5 min by heating with microwaves in a nitrogen atmosphere. The modified alumina powder comprising modified alumina particles obtained by the method is also provided.

Description

  The present invention relates to a method for producing alumina particles having an AlN modified layer, wherein a modified layer made of aluminum nitride is formed on at least a part of the surface of the alumina particles, and the modified alumina particles obtained thereby It relates to a modified alumina powder comprising

Alumina (Al ₂ O ₃ ) is a material with insulating properties and excellent thermal conductivity. For example, it is used as a refractory for various brick materials and as a ceramic material. It is mainly used as an inorganic filler material that is added to various resins to give various functions. Among them, it is well known as a thermally conductive filler in the manufacture of electronic devices such as semiconductor substrates and semiconductor packages, such as being added to a sealing material such as an epoxy resin.

  Alumina powders, such as those using the Bayer method and those using the spraying method, already have some production methods, and various studies have been made on the method of controlling the particle size and shape, It is also possible to make alumina particles of arbitrary shapes.

  On the other hand, aluminum nitride (AlN) is known as a material that is more excellent in thermal conductivity than alumina. The thermal conductivity of alumina is about 3 to 5 W / mK, whereas that of aluminum nitride is about 320 W / mK in theory, which is an order of magnitude larger than that of alumina. In view of this, there has been proposed a technique (see Patent Document 1) in which an aluminum nitride sintered body is pulverized and an aluminum nitride powder having an average particle diameter exceeding 50 μm is filled in a resin.

  However, aluminum nitride has been mainly used as a sintered body raw material so far, and is a typical production method such as an alumina reduction method (heating a mixed powder of alumina and carbon in nitrogen) or a direct nitriding method ( In the case of directly reacting metal aluminum powder and nitrogen, only fine particles of about several μm can be obtained. Therefore, it is difficult to obtain a material having a particle size of 10 μm or more necessary as an inorganic filler material, and it is difficult to obtain a material having a wide particle size distribution or high spherical aluminum nitride particles. The use as is not progressing.

  In addition, as an alumina reduction method in the production of aluminum nitride, typically, a mixture of ultrafine alumina particles having a particle size of 0.5 μm or less and graphite powder obtained by pulverizing graphite is placed in a crucible, under a nitrogen stream, There has been reported a method for synthesizing 0.2 to 0.4 μm of aluminum nitride close to the particle size of alumina ultrafine particles by heating at a temperature of 1600 ° C. or higher for 2 hours and holding at that temperature for 4 hours ( Non-patent document 1).

JP 2001-158610 A

Toshikazu Sakai and Jun Iwata, “Synthesis of AlN by Alumina Reduction”, 1974, Journal of the Ceramic Industry Association, Vol. 82, No. [3], p.

  Under such circumstances, the present inventors have made extensive studies aiming at the development of a new inorganic filler material utilizing the characteristics of aluminum nitride, and as a result, alumina powder comprising alumina particles having a predetermined particle diameter. , By performing a heat treatment with microwaves in a nitrogen atmosphere, at least a part of the surface of the alumina particles contained in the alumina powder was successfully modified to aluminum nitride, and the obtained was Since it was confirmed that the thermal conductivity of the alumina particles alone was far superior to that of the alumina particles alone, the present invention was completed.

  Therefore, an object of the present invention is to provide an alumina with an AlN modified layer that forms a modified layer made of aluminum nitride (AlN) on at least a part of the surface of the alumina particle to obtain modified alumina particles. The object is to provide a method for producing particles.

  Another object of the present invention is to provide a modified alumina powder comprising modified alumina particles in which a modified layer made of aluminum nitride (AlN) is formed on at least a part of the surface of the alumina particles. is there.

  That is, in the present invention, an alumina powder composed of alumina particles having a particle diameter of 7 μm or more and a carbon dispersion in which carbon is dispersed are kneaded, and the alumina powder to which carbon is adhered is heated by microwaves in a nitrogen atmosphere. An AlN modified layer is provided, wherein a modified layer made of aluminum nitride is formed on at least a part of the surface of the alumina particles by heat treatment held at a temperature of 1400 ° C. or higher and 1700 ° C. or lower for 5 minutes or longer. This is a method for producing alumina particles.

  The present invention also provides a modified alumina powder characterized by comprising alumina particles provided with an AlN modified layer obtained by the above method.

  In the method for producing alumina particles having an AlN modified layer in the present invention (hereinafter sometimes simply referred to as “modified alumina particles”), alumina powder made of alumina particles having a particle diameter of 7 μm or more is used. If the particle diameter is smaller than this, the alumina particles are likely to aggregate, and powder handling (transport) is difficult, and the filling property as a filler is also inferior, which is not practical. In addition, the use of alumina powder made of alumina particles having such a particle size is in consideration of the synthesis reaction of AlN used in the present invention, as will be described later. That is, when the particle size of the alumina particles is less than 7 μm, most of the alumina particles become aluminum nitride, and as a result, they are separated and produced into fine AlN and alumina of about 2 to 3 μm smaller than the initial particles. For this reason, the desired modified alumina particles cannot be obtained.

Further, considering that the powder composed of the modified alumina particles obtained in the present invention is used as a heat conductive filler by filling a resin, for example, the alumina powder preferably has an average particle diameter (D ₅₀ ). Is preferably 10 μm or more. Incidentally, the alumina filler generally used has an average particle diameter of 25 to 50 μm. This average particle diameter (D ₅₀ ) refers to a particle diameter corresponding to a cumulative percentage of 50% on a mass basis determined by a laser diffraction method. Further, the maximum particle size of the alumina particles contained in the alumina powder may be determined depending on the use of the obtained modified alumina particles. For example, it is mixed with an epoxy resin or the like and used as a heat conductive filler of an IC sealing material. Assuming such a case, the particle diameter of the alumina particles is desirably 80 μm or less. In addition, it does not restrict | limit especially about the manufacturing method of the alumina powder used by this invention, For example, what was manufactured by well-known methods, such as what was obtained using the buyer method, and what used the thermal spraying method, is used. be able to. In addition, when using alumina powder made of alumina particles having a particle diameter of 7 μm or more, for example, a sieve having an opening of 7 μm may be used to exclude undersieving.

In the method for producing modified alumina particles in the present invention, a carbon dispersion liquid in which carbon is dispersed is used and kneaded with the above alumina powder so that the carbon is adhered to the alumina powder. At this time, it is preferable that carbon is uniformly adhered to the surface of the alumina particles forming the alumina powder by sufficiently kneading. As described above, regarding the reason why carbon is adhered to alumina powder, in the method employed in the present invention, in order to modify at least a part of the surface of alumina particles to aluminum nitride, first, Al ₂ O ₃ and carbon (C ) To form Al ₄ O ₄ C or Al ₂ OC, and further generate Al ₂ O gas at a high temperature of microwave heating, which reacts with nitrogen gas to produce AlN. This is for thinking. At this time, as in Non-Patent Document 1, the present invention does not aim to obtain AlN particles by synthesizing AlN from alumina, but at least part or all of the surface of the alumina particles is modified with aluminum nitride. Therefore, an object of the present invention is to form a modified layer made of aluminum nitride on the surface layer portion while leaving the alumina particles as nuclei. Therefore, before the heat treatment as described in detail below, the alumina powder and the carbon dispersion are sufficiently kneaded so that the carbon is uniformly attached to the alumina particles forming the alumina powder. The above reaction is allowed to proceed with the carbon adhering to the surface so that only the surface layer portion is modified to AlN.

  The carbon dispersed in the carbon dispersion is preferably carbon fine particles, and more preferably carbon fine particles having a particle size of 0.01 μm or more and 0.1 μm or less. The carbon to be dispersed in the carbon dispersion liquid may be any of carbon black, cocoon, natural origin and industrially produced carbon. The carbon dispersion liquid may include a surfactant, a dispersion An agent, a resin such as glue, a preservative, and other additives may be included. As such a carbon dispersion, black ink can be suitably used in the present invention. At that time, it is desirable to add a carbon dispersion so that the alumina powder is in a slurry state so that carbon is uniformly attached to the surface of the alumina particles forming the alumina powder. In addition, when kneading the alumina particles and the carbon dispersion liquid, a known ball mill or the like can be used. In order to make carbon adhere uniformly to the surface of the alumina particles, it is preferable to use a ball mill. And kneading for about 10 minutes to 60 minutes.

And in this invention, the heat processing which hold | maintains the alumina powder which adhered carbon for 5 minutes or more in nitrogen atmosphere in the state made into the heating temperature of 1400 degreeC or more and 1700 degrees C or less using a microwave is performed. As explained above, the alumina particles having carbon adhered to the surface thereof by mixing with the carbon dispersion liquid absorb the microwaves by this heat treatment, and the solid phase reaction with Al ₂ O ₃ occurs. proceed. At that time, Al ₄ O ₄ C or Al ₂ OC is generated, and further, Al ₂ O gas is generated by heating with microwaves, which reacts with nitrogen (N ₂ ), and is more stable aluminum nitride (AlN). Thus, the surface of Al ₂ O ₃ is considered to be modified.

In the above heat treatment, when heating by microwaves is less than 1400 ° C., Al ₂ O gas is not generated, so it is considered that the above nitriding reaction does not occur even in a nitrogen atmosphere. Therefore, in the present invention, the alumina powder to which carbon is adhered is heat-treated at 1400 ° C. or higher by microwaves. When heating by microwaves exceeds 1700 ° C., AlN particle growth begins to occur, and the modified AlN layer peels off due to the difference in thermal expansion from the core alumina particles, or the fine AlN particles and the alumina particles become separated. There is a risk that they may be formed separately. Therefore, the upper limit of temperature is 1700 ° C.

  In addition, if the heat treatment is held for less than 5 minutes, the nitriding reaction may not be complete, so that the nitriding reaction should be held for 5 minutes or longer in order to sufficiently proceed. If the holding time is 5 minutes or more, the nitriding reaction is completed, and conversely, if held for a long time, the growth of AlN particles may be promoted, so the holding time is preferably 60 minutes or less. During this heat treatment, the temperature may be kept constant, or the temperature may be changed by changing the output of the microwave, but the temperature of the heat treatment is in the range of 1400 ° C. to 1700 ° C. Like that.

  The atmosphere for the heat treatment is not particularly limited as long as it is a nitrogen atmosphere in which a nitrogen source is present when the alumina powder to which carbon is attached is heat-treated. For example, a predetermined reaction chamber is filled with nitrogen in advance. Alternatively, heat treatment may be performed in a nitrogen stream while supplying nitrogen. The amount of nitrogen necessary for modifying the surface of the alumina particles with aluminum nitride may be set according to the thickness of the AlN modified layer to be formed. That is, the thickness of the AlN modified layer should be 0.1 μm or more, preferably 0.1 μm to 2 μm or less, more preferably 0.1 μm to 1 μm or less. If the thickness of the AlN modified layer is at least 0.1 μm, it will contribute sufficiently to the improvement of thermal conductivity in consideration of the use as a filler. When the thickness of the AlN modified layer exceeds 2 μm, the growth of the AlN particles as described above proceeds, or due to the difference in thermal expansion from the alumina particles as the core, the surface of the alumina particles is cooled to the room temperature. There is a possibility that the AlN particles may be separated and produced.

After the heat treatment as described above, when the mixture is allowed to cool to room temperature, a gray powdery reaction product is obtained. This reaction product is partially agglomerated and confirmed to be agglomerated, but the obtained reaction product particles have substantially the same shape as the alumina particles that make up the alumina powder used as the raw material. Recovered in state. When some of the particles of the obtained reaction product are observed using EPMA (Electron Probe Micro Analyzer) or the like, AlN having a thickness of about 0.1 μm to 1 μm exists on the surface of Al ₂ O ₃ . Is confirmed. Some of the obtained particles of the reaction product are covered with the modified AlN on the surface of the alumina particles, and some of the particles are not completely covered and the surface of the alumina particles is partially exposed. . This is the part of the alumina particles where the surface of the alumina particles could not be completely covered with carbon when the alumina powder and the carbon dispersion were kneaded before the heat treatment, and the carbon could not be adhered. Conceivable. In the present invention, not only the surface of the alumina particles are all coated with the AlN modified layer, but also the coating that is not completely covered and the surface of the alumina particles is partially exposed is the modified alumina particles. included. Even if the coating with the AlN layer is not complete, if the AlN modified layer is provided on a part of the surface of the alumina particles, for example, a resin made of such modified alumina particles is filled into a resin. When used as a thermally conductive filler, heat is conducted through a portion (AlN modified layer) excellent in thermal conductivity, so there is no problem.

  Further, it is preferable that the modified alumina particles of the present invention obtained by the heat treatment are further fired in the atmosphere at a temperature of 600 ° C. or higher and 800 ° C. or lower. By this firing treatment, carbon (C) remaining in the obtained modified alumina particles can be removed.

  According to the method of the present invention, a modified alumina particle can be obtained by forming an AlN modified layer made of aluminum nitride on at least a part of the surface of the alumina particle. The modified alumina particles obtained by the present invention are far superior in thermal conductivity than Al alumina particles alone due to AlN present on the surface, and substantially inherit the particle size and shape of the core alumina particles. Therefore, the modified alumina powder composed of such modified alumina particles can be suitably used as an inorganic filler material. In addition, it can be applied to various uses where alumina powder has been used so far, and it can also be expected to be used for new uses and to develop new materials.

FIG. 1 is a schematic diagram for explaining the outline of the microwave heating apparatus used for the heat treatment of Example 1. FIG. FIG. 2 is a graph showing the state of the measured temperature measured with a thermocouple until the heat treatment in Example 1 is completed. FIG. 3 is a powder X-ray diffraction result of the reaction product obtained in Example 1. 4 shows SEM-EPMA observation results of the reaction product obtained in Example 1. FIG. FIG. 5 is a graph showing the state of the measured temperature measured with a thermocouple until the heat treatment in Comparative Example 1 is completed. FIG. 6 is a powder X-ray diffraction result of the reaction product obtained in Comparative Example 1.

  EXAMPLES Hereinafter, although this invention is demonstrated in detail based on an Example etc., this invention is not restrict | limited to the content of the following Examples.

[Example 1]
As alumina powder, spherical alumina powder AX10-32 manufactured by Micron Corporation was used. This alumina powder has a 50% by mass average particle size (D50) determined on a mass basis using a laser particle size distribution analyzer (CILAS-920 manufactured by CILAS) of 10 μm, and a particle size distribution including a particle size of 7 μm to 11 μm. And consisting of Al ₂ O ₃ particles having a purity of 99.8% by mass. Moreover, the specific surface area calculated | required using the specific surface area measuring apparatus (BET method) is 0.28 m < ² > / g.

  After removing particles having a particle diameter of less than 7 μm with an ultrasonic vibration sieve using a sieve having a sieve mesh of 7 μm, 50 g of the alumina powder was weighed and put into a Teflon (registered trademark) container. Next, as a carbon dispersion, 10 g was added to the Teflon (registered trademark) container using a commercially available ink (made by Kuretake Seisho, ordinary concentration, ultrafine particle type), and kneaded by hand in a slurry state. Then, it was dried in a 120 ° C. dryer for 24 hours. In addition, when the said ink was put into an evaporating dish independently and it dried and the amount of solid content was calculated | required, it was confirmed that a 10.3 mass% solidified body is obtained.

  The mixture of the alumina powder and the carbon dispersion liquid dried for 24 hours was kneaded and crushed for 30 minutes with a ball mill (AV-2 type, manufactured by Asahi Rika Seisakusho). In the mixture immediately after drying, a plate-like material in which the glue component of the ink was thought to be solidified was confirmed. Was recovered for use in the next heat treatment. By the way, when 10 g was extracted from this powdery kneaded product and calcined at 600 ° C. in the atmosphere, the mass after calcining was 9.8 g. % Of alumina powder with carbon equivalent) was recovered.

  Next, 45 g of the powdery kneaded material (carbon-attached alumina powder) prepared above was placed in an alumina crucible (inner diameter 50 mmφ, height 55 mm) made of Toda refractory (thickness of the powdered kneaded material housed in the crucible) Was about 15 mm), and the following heat treatment was performed using a microwave heating apparatus as shown in FIG. Here, the microwave heating apparatus used for the heat treatment is such that a microwave oscillation body comprising a 2.45 GHz microwave oscillator 1, a power motor 2, and a 3-stab. Tutor is provided in a steel applicator 4. The applicator 4 accommodates an alumina crucible 7 in which carbon-attached alumina powder 6 is placed. The entire circumference of the alumina crucible 7 is surrounded by three layers of 25 mm thick ceramic fibers 8 having heat resistance for 1600 ° C. The inside of the alumina crucible 7 is filled with nitrogen gas from the outside of the applicator 4. Is connected to an alumina pipe 5 for nitrogen gas insertion. Furthermore, a sheath-type thermocouple 9 is attached from the outside of the applicator 4 so that the temperature of the carbon-attached alumina powder put in the crucible 7 can be grasped.

The microwave oscillator 1 was used to irradiate the microwave oscillator 1 with 1.2 kW of microwave while supplying nitrogen (N ₂ ) from the alumina pipe 5 at a rate of 5 L / min. And when it irradiated with the microwave for 40 minutes, the thermocouple 9 which shows the temperature of the carbon adhesion alumina powder displayed 1400 degreeC, and heat processing which hold | maintains this state for further 5 minutes was performed. During the heat treatment for 5 minutes, the microwave oscillation main body was adjusted so that the temperature of the carbon-adhered alumina powder was maintained at 1400 ° C. After the heat treatment for 5 minutes, the microwave oscillation was stopped and the furnace was cooled. FIG. 2 is a graph showing the state of the measured temperature measured with a thermocouple until the heat treatment in Example 1 is completed.

When the temperature in the alumina crucible reached room temperature, the reaction product after the heat treatment was taken out from the alumina crucible. As a result, 42 g of a powder that was gray and partially agglomerated was recovered. A part of the recovered reaction product was analyzed by powder X-ray diffraction. For the measurement, M18Xce manufactured by Mac Science Co., Ltd., CuKα ray as irradiation X-ray, voltage 40 kV, current 200 mA, scanning range: 2θ (diffraction angle) = 5 to 95 °, and scanning speed 5 ° / min. Performed under conditions. The results are shown in FIG. As can be seen from the results shown in FIG. 3, no carbon (C) was observed, and only peaks attributable to Al ₂ O ₃ and AlN were confirmed. Further, when all the recovered reactants were further baked at 600 ° C. for 4 hours in the atmosphere, the mass was reduced by 0.1% by mass.

The reaction product after baking was embedded in an epoxy resin, cut with a diamond cutter, and then polished to prepare an observation sample. SEM-EPMA observation was performed as follows. JXA8100 manufactured by JEOL Ltd. was used for the observation, under the conditions of an acceleration voltage of 15 kV, an irradiation current of 1.989 × 10 ⁻⁸ A, and 3000 times. And line analysis was performed simultaneously with element mapping by EMPA. The results are shown in FIG. As can be seen from the mapping result of N (nitrogen) and Al (aluminum) shown in FIG. 4, the modified layer containing nitrogen is 100 to 1000 nm on the surface of the alumina particles having a particle diameter of about 7 to 10 μm. It can be confirmed that it is formed to some extent. Moreover, according to the line analysis result, since an N peak exists at a position corresponding to the surface of the alumina particles, it was confirmed that the AlN modified layer was formed on the surface of the alumina particles.

  From the above results, according to Example 1, modified alumina particles provided with an AlN modified layer made of aluminum nitride on the surface of the alumina particles were obtained, and the reaction product recovered from the alumina crucible after the heat treatment was as described above. It was found to be a modified alumina powder composed of modified alumina particles.

[Comparative Example 1]
45 g of a powdery kneaded material (carbon-attached alumina powder) prepared in the same manner as in Example 1 was placed in an alumina crucible, and 5 L of nitrogen (N ₂ ) was added from the alumina pipe 5 using the same microwave heating apparatus as in Example 1. While supplying at a rate of / min, the microwave oscillator 1 was irradiated with 1.2 kW of microwave. When the microwave was irradiated for 40 minutes, it was confirmed that the thermocouple 9 displayed 1400 ° C., and at that time, the microwave oscillation was immediately stopped and the furnace was cooled, and a heat treatment was held at 1400 ° C. for 5 minutes. The reaction product was recovered in the same manner as in Example 1 except that it was not performed. FIG. 5 is a graph showing the state of the measured temperature measured with a thermocouple until the heat treatment in Comparative Example 1 is completed. It can be seen that the heating by the microwave shows a temperature rise behavior with good reproducibility, and the temperature curve is substantially the same as in Example 1 until the microwave is irradiated for 40 minutes.

When the temperature in the alumina crucible reached room temperature, the reaction product after the heat treatment was taken out from the alumina crucible. As a result, 44.8 g of a powdery product that was gray and partially agglomerated was recovered. Compared to the case of Example 1, little mass loss was observed. When a part of the recovered reaction product was analyzed by powder X-ray diffraction in the same manner as in Example 1, as shown in FIG. 6, only the peak attributed to Al ₂ O ₃ appeared, and the presence of carbon and AlN was It was not confirmed.

[Comparative Example 2]
Instead of the microwave oscillation main body and the applicator 4, heat treatment was performed with a heating apparatus using an electric furnace capable of adjusting the atmosphere. 45 g of the powdery kneaded material (carbon-attached alumina powder) prepared in the same manner as in Example 1 was placed in an alumina crucible, this crucible was placed in an electric furnace, and nitrogen (N ₂ ) was fed from the alumina pipe 5 at a rate of 5 L / min. Was heated until the temperature of the carbon-adhered alumina powder in the crucible reached 1450 ° C., and held at that temperature for 30 minutes. Thereafter, the reactor was cooled, and the reaction product was recovered in the same manner as in Example 1.

When the temperature in the alumina crucible became room temperature, it was taken out and the reaction product after heat treatment from alumina crucible, exhibit gray, in powder state containing the aggregated mass part is 44.9g recovered, Compared with the case of Example 1, almost no mass reduction was observed. When a part of the recovered reaction product was analyzed by powder X-ray diffraction in the same manner as in Example 1, only the peak attributed to Al ₂ O ₃ appeared, and the presence of carbon and AlN was not confirmed.

[Evaluation of thermal conductivity]
In order to evaluate the thermal conductivity of the modified alumina powder obtained in Example 1, the thermal conductivity was measured as follows. First, at room temperature, imidazole (trade name 2P4MZ: 2-ethyl-4-methylimidazole manufactured by Shikoku Kasei Co., Ltd.) is used as a curing agent with respect to 10 g of a bisphenol F type epoxy resin (YDF-170 manufactured by Toto Kasei Co., Ltd.). 0.1 g was added and mixed well in an agate mortar. The modified alumina powder obtained in Example 1 was blended to 50 vol% with respect to 0.25 g of the obtained mixture, and well mixed in an agate mortar. Next, defoaming treatment is performed, put into a mold (φ12.5 mm, thickness 1 mm), curing treatment at 150 ° C. for 3 hours and 200 ° C. for 8 hours in a high temperature furnace, cooling to room temperature, and a test piece Was made. For comparison purposes, instead of the modified alumina powder, the alumina powder used as a raw material in Example 1 (spherical alumina powder AX10-32 manufactured by Micron) was blended so as to be 50 vol%, and the above A test piece was prepared in the same manner as described above.

  About two types of test pieces prepared above, the thermal conductivity was measured by the laser flash method, respectively. In that case, the density of the material which comprises a test piece is needed when calculating heat conductivity. For the modified alumina powder obtained in Example 1, the thickness of the aluminum nitride phase on the surface of the alumina particles was estimated from the results of the above-described SEM-EDX line analysis, and the thickness was used to calculate the theory of alumina and aluminum nitride. From the density, the density of the modified alumina powder was 3.27. The density of the alumina powder was 3.98, and the density of the epoxy resin containing the curing agent was 1.10. As a result, the overall thermal conductivity of the test piece was 1.2 W / mk when the alumina powder was blended, whereas it was 1.4 W when the modified alumina powder obtained in Example 1 was blended. An improvement in thermal conductivity of about 16% was observed.

1: Microwave Oscillator 2: Power Motor 3: 3-stab. Tutor 4: Applicator 5: Nitrogen Gas Inserting Alumina Pipe 6: Alumina Powder Adhering to Carbon 7: Alumina Crucible 8: Ceramic Fiber 9: Sheath Type Thermocouple

Claims (7)

  Alumina powder composed of alumina particles having a particle diameter of 7 μm or more and a carbon dispersion in which carbon is dispersed are kneaded, and the alumina powder to which carbon is adhered is heated by microwaves in a nitrogen atmosphere to 1400 ° C. or more and 1700 ° C. A method for producing alumina particles provided with an AlN modified layer, characterized in that a modified layer made of aluminum nitride is formed on at least a part of the surface of the alumina particles by a heat treatment held at the following temperature for 5 minutes or more. .   The method for producing alumina particles having an AlN modified layer according to claim 1, wherein the carbon contained in the carbon dispersion is carbon fine particles having a particle size of 0.01 µm or more and 0.1 µm or less. Alumina powder average particle diameter (D ₅₀₎ is the 10μm or more, a manufacturing method of the alumina particles having an AlN reforming layer according to claim 1 or 2.   The manufacturing method of the alumina particle | grain provided with the AlN modified layer in any one of Claims 1-3 provided with the aluminum nitride modified layer of thickness 0.1 micrometer or more in at least one part of the surface of an alumina particle.   The AlN modified layer according to any one of claims 1 to 4, wherein the modified layer made of aluminum nitride is formed on the surface of the alumina particles and then fired in the atmosphere at a temperature of 600 ° C or higher and 800 ° C or lower. A method for producing alumina particles.   A modified alumina powder comprising alumina particles provided with an AlN modified layer obtained by the method according to any one of claims 1 to 5.   The modified alumina powder according to claim 6, which is used as a thermally conductive filler by filling a resin.