TWI597312B - Coated magnesia powder and its manufacturing method - Google Patents

Description

Coated magnesium oxide powder and method for producing same

The present invention relates to a coated magnesium oxide powder which can be used as a filler for a resin, and a method for producing the same. Further, the present invention relates to a resin composition comprising the above coated magnesium oxide powder, and a heat dissipating member comprising the resin composition.

The electronic device is composed of an electronic component such as a laminate, a printed wiring board, or a multilayer wiring board. In electronic parts, a resin composition is usually used for a prepreg, a spacer, a sealant, an adhesive sheet, etc., so that various properties or characteristics are required for the resin composition. For example, as a recent trend, mounting of a large-capacitance power element in an electronic device and high-density mounting have occurred, and the resin composition and its application products are required to have superior heat dissipation and moisture resistance as compared with the prior art.

The filler (filler) used for the resin composition for semiconductor sealing has been conventionally used as silica or alumina. However, since the thermal conductivity of cerium oxide is low, heat dissipation corresponding to an increase in heat generation due to high integration, high power, and high speed is not sufficient, and thus it is generated in terms of stable operation of semiconductors and the like. problem. On the other hand, when alumina having a thermal conductivity higher than that of cerium oxide is used, the heat dissipation property is improved. However, since the hardness of alumina is high, the abrasion of the kneading machine or the molding machine and the mold becomes severe.

Therefore, the industry has studied magnesium oxide having a thermal conductivity higher than that of cerium oxide and having a thermal conductivity of about 2 times that of alumina as a material for a semiconductor sealing resin filler. However, the magnesium oxide powder has a hygroscopicity greater than that of the cerium oxide powder. Therefore, when the magnesium oxide powder is used as a resin sealing material for semiconductor sealing, there is a problem in that the absorbed water hydrates with the magnesium oxide to expand the volume of the filler, thereby causing cracks, Reduced thermal conductivity, etc. Therefore, imparting moisture resistance to the magnesium oxide powder used as the resin sealing material for semiconductor sealing has become a major problem in securing stable operation of the semiconductor for a long period of time.

As a method for improving the moisture resistance of the magnesium oxide powder, Patent Document 1 and Patent Document 2 disclose a method for producing a coated magnesium oxide powder, which is characterized in that an aluminum salt or a cerium compound is mixed with a magnesium oxide powder, and is separated by filtration. The solid component is dried and calcined, whereby the surface of the magnesium oxide powder is coated with a coating layer comprising aluminum or a composite oxide of cerium and magnesium.

Prior technical literature

Patent literature

Patent Document 1: Japanese Patent Laid-Open Publication No. 2003-34522

Patent Document 2: Japanese Patent Laid-Open Publication No. 2003-34523

However, although the moisture-retaining property of the coated magnesium oxide powder obtained by the above method is improved, the powder particles have an angular shape, so that the filling property to the resin is low, and the fluidity of the obtained resin composition is improved. Low problem.

An object of the present invention is to solve the above-mentioned problems, and to provide an oxide which is excellent in thermal conductivity and moisture resistance and which is used as a filler for a resin, and which has high fluidity after filling, and is excellent in formability. Powder and its method of manufacture. Another object of the present invention is to provide a resin composition comprising the coated magnesium oxide powder and a heat dissipating member comprising the resin composition.

The present invention relates to a coated magnesium oxide powder characterized by having a magnesium oxide powder which exhibits a void amount in a particle of 0.3 to 0.8 cm ³ /g and a minimum particle diameter of 0.2 in a mercury intrusion pore distribution. And the coating layer is at least a part of the surface of the magnesium oxide powder, and is composed of a magnesium phosphate compound; and the phosphorus content in the coated magnesium oxide powder is 0.1. ~10% by mass.

Further, the present invention relates to a filler which is composed of the coated magnesium oxide powder.

Furthermore, the present invention also relates to a resin composition comprising a resin and the filler. The resin composition can be used as a heat dissipating member such as an adhesive or a semiconductor encapsulant.

Further, the present invention relates to a method for producing a coated magnesium oxide powder, which comprises calcining at 100 to 1000 ppm B, 300 ppm or less Na, 300 ppm or less K, 0.02 to 0.5 by firing at 1000 ° C to 1200 ° C. And the mass% of the Cl, and the magnesium oxide having a purity of 98% or more in terms of SiO ₂ of 0.02 to 0.5% by mass and Ca of 0.1 to 0.8% by mass of CaO is obtained, and after the magnesium oxide powder is obtained, the above The magnesium oxide powder is mixed with the phosphorus compound and calcined at 300 ° C or higher to form a coating layer composed of the magnesium phosphate compound on at least a part of the surface of the magnesium oxide powder.

According to the present invention, it is excellent in thermal conductivity and moisture resistance, and is excellent in filling property when used as a filler for a resin, and the fluidity of the resin composition after filling is high, and as a result, coating oxidation excellent in formability is obtained. Magnesium powder.

Fig. 1 is an electron micrograph obtained by photographing the coated magnesium oxide powder produced in Example 1.

Hereinafter, the present invention will be specifically described.

The coated magnesium oxide powder of the present invention has a magnesium oxide powder exhibiting specific physical properties and a coating layer composed of a magnesium phosphate-based compound formed on the surface thereof. The coating layer composed of the magnesium phosphate-based compound may be formed on the entire surface of the magnesium oxide powder, or may be formed only on one part of the surface of the magnesium oxide powder. The surface of the magnesium oxide powder not covered by the coating layer composed of the magnesium phosphate-based compound can be exposed.

In the present invention, the magnesium oxide powder satisfies the amount of voids in the particles of 0.3 to 0.8 cm ³ /g, the most frequent particle diameter of 0.2 to 1.0 μm, and the inflection point diameter of 0.9 μm or more. The coated magnesium oxide powder of the present invention can be suitably used as a thermal conductive filler by forming a coating layer composed of a magnesium phosphate compound on the surface of such a magnesium oxide powder.

Further, each measured value is a value measured in a mercury intrusion type pore distribution measuring device.

The inflection point diameter and the amount of voids in the particle can be obtained from the cumulative pore volume curve. In the cumulative pore volume curve, the vertical axis represents the pore volume of the particles sequentially determined from the larger pore per unit weight of the sample. The cumulative value is the cumulative pore volume, and the horizontal axis represents the pore diameter.

The so-called inflection point is the point at which the cumulative pore volume curve rises sharply. According to the measurement sample, the number of inflection points is not limited to one, and there are a plurality of cases, but the inflection point at which the pore diameter is the largest is set as the inflection point of the present invention. The recurve point diameter is the pore diameter of the inflection point.

If the recursive spot diameter is less than 0.9 μm, the amount of fine particles increases, so that an imminent increase in viscosity occurs when it is filled into the resin. Preferably, the inflection point diameter is 0.9 to 1.5 μm.

The amount of voids in the particles is smaller than the amount of voids of agglomerated particle diameters present in the particles, and the amount of voids in the particles is the total pore volume expressed by the cumulative pore volume in the pore diameter of 0.003×10 ^-6 to 100×10 ^-6 m. The volume obtained by subtracting the cumulative pore volume in the above-mentioned inflection point is expressed.

When the amount of voids in the particles of the magnesium oxide powder is less than 0.3 cm ³ /g, the voids in the particles are small, and a sufficient amount of the resin is not impregnated into the particles, and the mechanical strength of the resin composition is deteriorated. Moreover, the thermal conductivity is also lowered. On the other hand, when the amount of voids in the particles exceeds 0.8 cm ³ /g, the voids in the particles are present deep in the particles, so that the resin does not sufficiently spread into the inside of the voids, and bubbles are generated between the particles and the resin to lower the thermal conductivity. Preferably, the amount of voids in the particles is from 0.3 to 0.7 cm ³ /g.

The most frequent particle size can be determined from the mercury intrusion pore distribution measurement, which is the pore diameter corresponding to the maximum value of the log differential pore volume distribution curve. In the case where the pore distribution of the magnesium oxide particles of the present invention is measured by a mercury intrusion measuring device, the most frequent particle diameter corresponds to the diameter of the gap between the magnesium oxide particles. If the most frequent particle diameter of the magnesium oxide powder is less than 0.2 μm, the amount of fine particles increases, so that an imminent increase in viscosity occurs when the resin is filled. On the other hand, if the most frequent particle diameter exceeds 1.0 μm, the amount of the larger particles increases, so the resin composition The mechanical strength deteriorates. Moreover, the thermal conductivity is also lowered. Preferably, the mode of the primary particle size is from 0.3 to 1.0 μm.

A coating layer composed of a magnesium phosphate-based compound is formed on the magnesium oxide powder. With the coating layer, the moisture resistance of the magnesium oxide powder can be improved. The magnesium phosphate-based compound is, for example, a compound represented by a composition formula: Mg _x P _y O _z (x = 1 to 3, y = 2, and z = 6 to 8).

Since the coated magnesium oxide powder of the present invention has a coating layer composed of a magnesium phosphate-based compound, phosphorus is contained as a constituent element. The content of phosphorus is 0.1 to 10% by mass based on the coated magnesium oxide powder of the present invention. Since the phosphorus is contained in such a range, the coated magnesium oxide powder of the present invention can be excellent in moisture resistance. When the content of phosphorus is less than 0.1% by mass, sufficient moisture resistance cannot be exhibited. On the other hand, when the content of phosphorus exceeds 10% by mass, the magnesium phosphate-based compound not only coats the surface of the magnesium oxide powder, but also the magnesium phosphate-based compound is formed into a single particle or the coating layer is too thick, so that the thermal conductivity is lowered.

The coated magnesium oxide powder of the present invention has an advantage of being excellent in filling property when filled in a resin and having high fluidity of the resin composition after filling, and therefore can be suitably formulated into a resin as a filler. The resin which can be used in the present invention is, for example, a thermosetting resin or a thermoplastic resin. The thermosetting resin is not particularly limited, and examples thereof include a phenol resin, a urea resin, a melamine resin, an alkyd resin, a polyester resin, an epoxy resin, a diallyl phthalate resin, and a polyaminocarboxylic acid. Ester resin, or polyoxyl resin. The thermoplastic resin is not particularly limited, and examples thereof include a polyamide resin, a polyacetal resin, a polycarbonate resin, a polybutylene terephthalate resin, a polyfluorene resin, a polyamidoximine resin, and a poly An ether quinone imine resin, a polyarylate resin, a polyphenylene sulfide resin, a polyetheretherketone resin, a fluororesin, or a liquid crystal polymer.

The amount of the magnesium oxide powder to be coated in the resin composition of the present invention is not particularly limited as long as it is appropriately determined depending on the properties required for the resin composition. but, As an example, it may be used in the range of 0.1 to 100 parts by mass of the coated magnesium oxide powder based on 100 parts by mass of the resin.

The resin composition containing the coated magnesium oxide powder of the present invention can be used in various fields depending on the characteristics of the resin. However, since the coated magnesium oxide powder of the present invention is excellent in thermal conductivity, it is particularly suitable for applications requiring heat dissipation. Further, the resin composition of the present invention can be used as a semiconductor sealing material excellent in thermal conductivity and moisture resistance.

Next, a method of producing the coated magnesium oxide powder of the present invention will be described.

First, magnesium oxide exhibiting specific physical properties is obtained by calcining magnesium hydroxide. Magnesium oxide exhibiting specific physical properties can be obtained by previously adjusting the concentration of each impurity element contained in the calcined magnesium hydroxide to a specific concentration and setting the temperature at the time of calcination to a range of 1000 to 1200 °C.

The different elements in the magnesium hydroxide are as follows. B (boron): 100 to 1000 ppm (preferably 300 to 800 ppm), Na (sodium): 300 ppm or less (preferably 200 ppm or less), K (potassium): 300 ppm or less (preferably 200 ppm or less), Cl (chlorine) ): 0.02 to 0.5% by mass (preferably 0.15 to 0.3% by mass), Si (矽): 0.02 to 0.5% by mass (0.05 to 0.15% by mass) in terms of SiO ₂ , and Ca: 0.1 to 0.8 in terms of CaO % by mass (preferably 0.2 to 0.5% by mass). Furthermore, the concentration adjustment of the different elements can be performed using previous methods. For example, when B is insufficient, boric acid or magnesium borate may be added for adjustment. When Cl is insufficient, hydrochloric acid or magnesium chloride may be added for adjustment. In the case where Si is insufficient, sodium citrate, magnesium citrate or calcium citrate may be added for adjustment. In the case of insufficient calcium, calcium hydroxide, calcium oxide, or calcium carbonate may be added for adjustment.

If B in the magnesium hydroxide exceeds 1000 ppm, or Na or K exceeds 300 ppm, the obtained magnesium oxide does not satisfy the conditions of the void amount and/or the inflection point diameter of the above particles. In addition, when Ca in the magnesium hydroxide is outside the range of 0.1 to 0.8% by mass in terms of CaO, or when Si is outside the range of 0.02 to 0.5% by mass in terms of SiO ₂ , the obtained magnesium oxide is obtained. The shape of the above-mentioned mode of the least-frequency and/or the radius of the inflection point is not satisfied, and the shape does not become a shape having a circular shape. As the magnesium hydroxide, it is preferred to use a purity of 98% or more.

Further, the temperature at which the magnesium hydroxide is calcined is preferably in the range of from 1,000 to 1,200 °C. If the calcination temperature is less than 1000 ° C, the obtained magnesium oxide does not satisfy the conditions of the intragranular void amount, the most frequent particle diameter, and/or the inflection point diameter. Further, when the calcination temperature exceeds 1200 ° C, the obtained magnesium oxide does not satisfy the above-described conditions of the most frequent particle diameter and/or the inflection point diameter. The calcination furnace and the calcination time are not particularly limited, and may be a calcination furnace in which magnesium hydroxide can be converted into magnesium oxide at the above temperature, and a calcination time.

Magnesium oxide obtained by calcining magnesium hydroxide as described above is coarsely pulverized by using a pulverizer as needed. Thereby, magnesium oxide powder can be obtained. The magnesium oxide powder is mixed with a phosphorus compound, and if necessary, dried at a temperature of about 120 ° C to 200 ° C, and then pulverized by a ball mill or the like to obtain a powder. The powder is calcined at 300 ° C or higher to obtain a magnesium oxide powder in which at least a part of the surface is formed with a coating layer composed of a magnesium phosphate compound.

The phosphorus compound is not particularly limited as long as it is a compound which can react with magnesium oxide to form a magnesium phosphate compound, and examples thereof include phosphoric acid, phosphate, and acid phosphate. These may be used alone or in combination of two or more. Preferred is an acid phosphate. Examples of the acid phosphate include isopropyl acid phosphate, 2-ethylhexyl acid phosphate, acid acid oleate, acid methyl phosphate, acid ethyl phosphate, and acid propyl phosphate. Butyl acid phosphate, Lauryl acid phosphate, stearyl phosphate.

The amount of the phosphorus compound to be used may be adjusted so that the content of phosphorus in the entire coated magnesium oxide powder such as the final product is 0.1 to 10% by mass. For example, the phosphorus compound can be used in an amount of about 5 to 10% by mass based on the magnesium oxide powder.

The temperature at the time of calcination is 300 ° C or more, preferably about 300 to 700 ° C. As an example, calcination is carried out at 500 ° C for 1 hour. By the calcination, the phosphorus compound is converted into a magnesium phosphate-based compound, whereby a coating layer composed of a magnesium phosphate-based compound can be formed on the surface of the magnesium oxide powder.

Example

Hereinafter, the present invention will be described in more detail by way of examples, but the invention is not limited by the examples.

(Measurement method of concentration of impurity elements)

After Ba and P were dissolved in an acid, the mass was measured using an ICP emission spectrometer (trade name: SPS-5100, manufactured by Seiko Instruments) to calculate the concentration in the sample.

In the case of Cl, the sample was dissolved in an acid, and the mass was measured using a spectrophotometer (trade name: UV-2550, manufactured by Shimadzu Corporation) to calculate the concentration in the sample.

For Si and Ca, the concentration in the sample was measured using a fluorescent X-ray apparatus (trade name: SPS-5100, manufactured by Seiko Instruments). Among them, the values are expressed in terms of SiO ₂ conversion and CaO conversion.

Regarding Na and K, the concentration in the sample was measured using an atomic absorption photometer (trade name: Z-2300, manufactured by Hitachi High-Technologies).

(BET specific surface area measurement method)

The specific surface area was measured by a gas adsorption method using a specific surface area measuring device (trade name: Macsorb 1210, manufactured by Mountech Co., Ltd.).

(Measurement of pore distribution)

Determination of pore distribution (recurve point diameter, intraparticle void volume, and most frequent particle size)

The void diameter (the most frequent particle diameter) corresponding to the maximum value of the 10 g differential pore volume distribution curve obtained by the mercury intrusion pore distribution measurement was determined under the following conditions. The mercury intrusion pore size measuring device was measured using an AutoPore 9410 manufactured by Micromeritics. Further, the mercury type is a special grade mercury reagent having a purity of 99.5 mass% or more and a density of 13.5335 × 10 ³ kg/m ³ . The measurement unit was a unit for powder samples having a unit internal volume of 5 × 10 ^-6 m ³ and a stem volume of 0.38 × 10 ^-6 m ³ . The measurement sample is precisely weighed in a range of 0.10×10 ^-3 to 0.13×10 ^-3 kg in a concentration of 0.1 mm × 10 ^-3 to 0.13 × 10 ^-3 kg in a 330 mesh standard sieve (JIS-R8801-87), and filled into the measurement unit. . After the measurement unit was attached to the apparatus, the inside of the unit was kept at a pressure of 50 μHg (6.67 Pa) or less for 20 minutes under reduced pressure. Next, mercury was filled in the measuring unit until the pressure became 1.5 psia (10342 Pa). Thereafter, mercury was injected at a pressure ranging from 2 psia (13790 Pa) to 60,000 psia (413.7 MPa), and the pore distribution was measured.

When the pressure of mercury intrusion is converted into a pore diameter, the following formula (I) (Washburn type) is used.

D=-(1/P). 4 γ. Cos Ψ (I)

Here, D: pore diameter (m); P: mercury intrusion pressure (Pa); γ: mercury surface tension (485 dyne.cm ^-1 (0.485 Pa.m)); Ψ: mercury contact angle (130 °=2.26893rad).

(Method for measuring moisture resistance)

A 10 g sample was weighed and placed in a shallow pan and placed in a constant temperature and humidity machine (85 ° C, 85 Rh%). After keeping in this state for one week, it was dried overnight in a dryer at 120 °C. After drying, the weight was weighed and the weight increase rate was calculated.

(Method for measuring thermal conductivity)

A sample of a high thermal conductivity resin composition having a diameter of 13 mm and a thickness of 2 mm which was completely cured by adding the resin of the present invention was prepared, and the thermal diffusivity was measured by a laser flash method in the range of 30 to 100 °C. The device used LFA-457 manufactured by NETZSCH. The specific heat was measured and the specific gravity was measured by the Archimedes method, and the thermal conductivity as a product of the thermal diffusivity and the specific heat and the density was calculated.

(Method for measuring melt flow rate)

The resin composition was measured in accordance with JIS-K7210 at a measurement temperature of 230 ° C and a load of 2.16 Kg.

(Method for producing resin composition)

The resin composition used in the measurement of the melt flow rate was prepared in the following order.

After 100 g of EEA (ethylene-ethyl acrylate copolymer) was melted, 333 g of a filler was added in small portions for about 10 minutes while observing the kneading state, and further kneading was carried out for 10 minutes. The roll spacing at this time was 0.5 mm.

After the kneading was completed, the composite was peeled off, and the recovered composite was cut into a size of about 5 mm square, and dried in a vacuum dryer at 90 ° C for 1 hour to prepare a sample for measuring a melt flow rate.

(Method for measuring the composition of a magnesium phosphate compound)

The composition of the magnesium phosphate-based compound coating layer was measured by an X-ray diffraction method using Cu-Kα ray using an X-ray diffraction apparatus (trade name: RINT-Ultima III, manufactured by Rigaku).

(Example 1)

Hydrogen having a purity of 99.2%, which is adjusted so that Ca is 0.23 mass% in terms of CaO, and SiO ₂ is 0.07 mass%, Cl is 0.16 mass%, B is 402 ppm, Na is 11 ppm, and K is 9 ppm. Magnesium oxide was calcined in an electric furnace at 1,100 ° C for 1 hour, thereby preparing magnesium oxide.

After the magnesium oxide was crushed by Power Mill, 5% by weight of isopropyl acid phosphate as an acid phosphate was added to magnesium oxide. Thereafter, the mixture was dried at 120 ° C for 2 hours, and then pulverized in a ball mill and calcined at 500 ° C for 1 hour to obtain a target coated magnesium oxide powder.

The concentration of the impurity element, the BET specific surface area, the pore distribution, the moisture resistance, the thermal conductivity, and the melt flow rate of the obtained coated magnesium oxide powder were measured based on the above method, and the results are shown in Table 1.

Further, the composition of the coating layer on the surface of the obtained coated magnesium oxide powder was measured by the above method, and it was found to be Mg ₂ P ₂ O ₇ .

Fig. 1 is an electron micrograph of the obtained coated magnesium oxide powder. The particle shape of the coated magnesium oxide powder is spherical. Here, the spherical powder refers to a powder composed of particles having a round shape without a horn, whereas the amorphous powder refers to a horn formed by combining a plurality of crystal grains. A powder composed of particles.

(Example 2)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the calcination temperature of the magnesium hydroxide was changed to 1175 °C. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 3)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that Ca was adjusted so that CaO was 0.48% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 4)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that Si was adjusted so that SiO ₂ was 0.12% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 5)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the B concentration of the magnesium hydroxide was adjusted to 700 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 6)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the Na concentration of the magnesium hydroxide was adjusted to 200 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 7)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the K concentration of the magnesium hydroxide was adjusted to 200 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 8)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the amount of the acid phosphate was changed so that the content of the phosphorus in the coated magnesium oxide powder was 0.18% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Example 9)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the amount of the acid phosphate was changed so that the content of the phosphorus in the coated magnesium oxide powder was 4.6% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 1.

(Comparative Example 1)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the calcination temperature of the magnesium hydroxide was changed to 950 °C. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 2)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the calcination temperature of the magnesium hydroxide was changed to 1400 °C. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 3)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the CaO concentration of the magnesium hydroxide was changed to 1% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 4)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the SiO ₂ concentration of the magnesium hydroxide was changed to 4% by mass. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 5)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the B concentration of the magnesium hydroxide was changed to 1200 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 6)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the Na concentration of the magnesium hydroxide was changed to 400 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 7)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the K concentration of the magnesium hydroxide was changed to 400 ppm. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 8)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the amount of the acid phosphate was changed to 0.058% by mass based on the total content of the phosphorus-coated magnesium oxide powder. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

(Comparative Example 9)

The coated magnesium oxide powder was obtained under the same conditions as in Example 1 except that the amount of the acid phosphate was changed to 12.1% by mass based on the total content of the phosphorus-coated magnesium oxide powder. The measurement of each physical property was carried out in the same manner as in Example 1. The results are shown in Table 2.

Claims (12)

A coated magnesium oxide powder having: magnesium oxide powder in a mercury intrusion pore distribution, exhibiting a void amount in the particle of 0.3 to 0.8 cm ³ /g, a most frequent particle diameter of 0.2 to 1.0 μm, and a reverse The meander diameter is 0.9 μm or more; and the coating layer is located on at least a part of the surface of the magnesium oxide powder, and has a composition formula: Mg _x P _y O _z (x=1~3, y=2, z=6~) 8) The magnesium phosphate compound represented by the above; the above-mentioned inversion point diameter system: the pore diameter under the inflection point where the pore diameter is the largest in the cumulative pore volume curve; and the void amount in the above-mentioned particle: from the pore diameter 0.003×10 ^{- The} volume of the total pore volume expressed by the cumulative pore volume in ⁶ to 100 × 10 ^-6 m minus the cumulative pore volume in the above inflection point; the above-mentioned MF range: the largest with the log differential pore volume distribution curve The value corresponds to the pore diameter; and the content of phosphorus in the coated magnesium oxide powder is 0.1 to 10% by mass. A filler material comprising the coated magnesium oxide powder of claim 1 of the patent application. A resin composition comprising a resin and a filler of the second aspect of the patent application. The resin composition of claim 3, wherein the resin is a thermosetting resin. The resin composition of claim 4, wherein the thermosetting resin is a phenol resin, a urea resin, a melamine resin, an alkyd resin, a polyester resin, an epoxy resin, a diallyl phthalate resin, Polyurethane resin, or polyoxyl resin. The resin composition of claim 3, wherein the resin is a thermoplastic resin. The resin composition of claim 6, wherein the thermoplastic resin is a polyamide resin, a polyacetal resin, a polycarbonate resin, a polybutylene terephthalate resin, a polyfluorene resin, or a polyamide. Imine resin, polyether oxime resin, polyarylate resin, polyphenylene sulfide resin, polyether ether ketone resin, or fluororesin. A heat dissipating member comprising the resin composition according to any one of claims 3 to 7. A method for producing a coated magnesium oxide powder, which comprises calcining at 100 to 1000 ppm B, 300 ppm or less Na, 300 ppm or less K, and 0.02 to 0.5 mass% Cl at 1000 ° C to 1200 ° C, and is converted into SiO ₂ is 0.02 to 0.5% by mass of Si, and magnesium hydroxide having a purity of 98% or more of Ca having 0.1 to 0.8% by mass of CaO is obtained, and after the magnesium oxide powder is obtained, the magnesium oxide powder and the phosphorus compound are mixed and 300. Calcination is carried out at a temperature above °C, whereby at least a part of the surface of the magnesium oxide powder is formed to contain phosphoric acid represented by a composition formula: Mg _x P _y O _z (x=1~3, y=2, z=6-8) A coating layer of a magnesium compound. The production method according to claim 9, wherein the phosphorus compound is at least one selected from the group consisting of phosphoric acid, phosphate, and acid phosphate. The manufacturing method of claim 10, wherein the phosphorus compound is selected from the group consisting of isopropyl acid phosphate, 2-ethylhexyl acid phosphate, acid acid phosphate, acid methyl phosphate, and acid phosphate. One or more acid phosphates of the group consisting of ethyl ester, propyl acid phosphate, butyl acid phosphate, lauryl acid phosphate, and stearyl phosphate. The production method according to any one of claims 9 to 11, wherein the phosphorus compound is used in such a manner that the content of phosphorus in the coated magnesium oxide powder is 0.1 to 10% by mass.