TWI736292B - Alumina powder, resin composition, heat dissipation member, and method for manufacturing coated alumina particles - Google Patents

Alumina powder, resin composition, heat dissipation member, and method for manufacturing coated alumina particles Download PDF

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TWI736292B
TWI736292B TW109117983A TW109117983A TWI736292B TW I736292 B TWI736292 B TW I736292B TW 109117983 A TW109117983 A TW 109117983A TW 109117983 A TW109117983 A TW 109117983A TW I736292 B TWI736292 B TW I736292B
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alumina
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alumina particles
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TW202104084A (en
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佐佐木修治
中園淳一
田上將太朗
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日商電化股份有限公司
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B21/00—Nitrogen; Compounds thereof
    • C01B21/06—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron
    • C01B21/072—Binary compounds of nitrogen with metals, with silicon, or with boron, or with carbon, i.e. nitrides; Compounds of nitrogen with more than one metal, silicon or boron with aluminium
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/20—Oxides; Hydroxides
    • C08K3/22—Oxides; Hydroxides of metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/28—Nitrogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L101/00—Compositions of unspecified macromolecular compounds

Abstract

An object of the invention is to provide alumina particles that can suppress any increase in viscosity when added to a resin, and realize high thermal conductivity for a resin composition containing that resin. The alumina powder of the invention contains coated alumina particles composed of alumina particles and a coating layer that coats the alumina particles, the coated alumina particles having an equivalent circle diameter of the projected area as measured by microscopy of at least 1 µm, wherein the coating layer contains aluminum nitride and the average sphericity of the coated alumina particles is at least 0.85 but not more than 0.97.

Description

氧化鋁粉末、樹脂組成物、散熱零件、以及被覆氧化鋁粒子之製造方法Alumina powder, resin composition, heat dissipation part, and manufacturing method of coated alumina particles

本發明關於氧化鋁粉末、樹脂組成物、散熱零件、及被覆氧化鋁粒子之製造方法。The present invention relates to a manufacturing method of alumina powder, resin composition, heat dissipation parts, and coated alumina particles.

近年，電氣設備的小型化及高性能化正進展。伴隨小型化及高性能化，構成電氣設備之電子零件的安裝密度變高，將電子零件所產生的熱有效地散出的必要性增高。In recent years, the miniaturization and high performance of electrical equipment are progressing. Along with miniaturization and higher performance, the mounting density of electronic components constituting electrical equipment has increased, and the need to effectively dissipate heat generated by electronic components has increased.

又，在可抑制環境負荷之電動車等的功率器件用途中，有時會有於電子零件施加高電壓，或流通大電流的情況。此時，會產生高熱量，為了應對產生的高熱量，比以往更有效地將熱散出的要求增高。作為用以對應如此之要求的技術，例如專利文獻1中揭示含有3種氧化鋁填料而成之樹脂組成物。又，專利文獻2中揭示含有球狀氧化鋁粒子與非球狀氧化鋁粒子之氧化鋁摻合粒子、及含有該粒子之樹脂組成物。另外，專利文獻3中就熱傳導性填料而言，揭示一種氮化鋁系粒子，具備由氧化鋁及氮氧化鋁中之至少一者構成之芯層、及形成於前述芯層之表面的厚度1.1μm以上之由氮化鋁構成之表面層。 [先前技術文獻] [專利文獻]In addition, in power device applications such as electric vehicles that can suppress environmental load, high voltage may be applied to electronic components or large current may flow. At this time, high heat will be generated, and in order to cope with the high heat generated, there is an increasing demand for more effective heat dissipation than before. As a technique for responding to such a demand, for example, Patent Document 1 discloses a resin composition containing three types of alumina fillers. In addition, Patent Document 2 discloses alumina blended particles containing spherical alumina particles and non-spherical alumina particles, and a resin composition containing the particles. In addition, as for the thermally conductive filler, Patent Document 3 discloses an aluminum nitride-based particle having a core layer composed of at least one of aluminum oxide and aluminum oxynitride, and a thickness of 1.1 formed on the surface of the core layer. Surface layer made of aluminum nitride above μm. [Prior Technical Literature] [Patent Literature]

[專利文獻1]日本特開2009-164093號公報 [專利文獻2]日本特開2009-274929號公報 [專利文獻3]日本特開2012-41253號公報[Patent Document 1] JP 2009-164093 A [Patent Document 2] JP 2009-274929 A [Patent Document 3] JP 2012-41253 A

[發明所欲解決之課題][The problem to be solved by the invention]

但是，專利文獻1及2中，由於氧化鋁粒子的比表面積高，平均球形度低，包含變形的形狀等理由，存有將氧化鋁粒子填充於樹脂時發生增黏，不易以高比例填充氧化鋁粒子的問題。因此，成形性低，又，獲得之散熱零件之熱傳導率亦低。However, in Patent Documents 1 and 2, due to the high specific surface area of the alumina particles, the low average sphericity, and the deformed shape, there are reasons such as the increase in viscosity when the alumina particles are filled in the resin, and it is difficult to fill and oxidize at a high ratio. The problem of aluminum particles. Therefore, the formability is low, and the thermal conductivity of the obtained heat dissipation part is also low.

又，專利文獻3中係藉由微波照射獲得氮化鋁系粒子，但該製法無法獲得球狀的粒子。故如上述，專利文獻3記載之氮化鋁系粒子的形狀亦差，因此存有將氧化鋁系粒子填充於樹脂時發生增黏，氮化鋁系粒子的高填充困難的問題。結果即使使用專利文獻3記載之氮化鋁系粒子，成形性亦低，又，獲得之散熱零件之熱傳導率低。In addition, in Patent Document 3, aluminum nitride-based particles are obtained by microwave irradiation, but this production method cannot obtain spherical particles. Therefore, as described above, the aluminum nitride-based particles described in Patent Document 3 are also poor in shape. Therefore, there is a problem that the aluminum nitride-based particles increase in viscosity when the alumina-based particles are filled in the resin, and the high filling of the aluminum nitride-based particles is difficult. As a result, even if the aluminum nitride-based particles described in Patent Document 3 are used, the formability is low, and the thermal conductivity of the obtained heat-radiating part is low.

本發明係鑒於如此之課題而成，旨在提供含有特定被覆氧化鋁粒子的氧化鋁粉末，填充於樹脂時可抑制黏度上升，且可達成含有該樹脂之樹脂組成物的高熱傳導化；以及提供含有該氧化鋁粉末的樹脂組成物、散熱零件、及被覆氧化鋁粒子之製造方法。 [解決課題之手段]The present invention is made in view of such problems, and aims to provide alumina powder containing specific coated alumina particles, which can suppress the increase in viscosity when filled with resin, and can achieve high thermal conductivity of the resin composition containing the resin; and A resin composition containing the alumina powder, a heat dissipating component, and a method for producing coated alumina particles. [Means to solve the problem]

本案發明人等為了達成上述目的而進行努力研究的結果，發現含有特定被覆氧化鋁粒子的氧化鋁粉末填充於樹脂時可抑制黏度上升，且能獲得藉由含有該氧化鋁粉末可達成高熱傳導化的樹脂組成物及散熱零件，而完成了本發明。As a result of diligent research by the inventors of the present invention to achieve the above-mentioned object, they have found that when an alumina powder containing specific coated alumina particles is filled in a resin, the increase in viscosity can be suppressed, and it can be achieved that high thermal conductivity can be achieved by containing the alumina powder. The resin composition and heat dissipating parts of, and completed the present invention.

亦即，本發明如下。 [1] 一種氧化鋁粉末，含有被覆氧化鋁粒子， 該被覆氧化鋁粒子具有氧化鋁粒子、及將前述氧化鋁粒子予以被覆之被覆層，且利用顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下； 前述被覆層含有氮化鋁； 前述被覆氧化鋁粒子之平均球形度為0.85以上0.97以下。 [2] 如[1]之氧化鋁粉末，其中，前述氧化鋁粉末之利用雷射繞射散射法獲得之體積基準頻率粒度分布中，於粒徑為2μm以上200μm以下之粒度範圍具有多個峰部。 [3] 如[1]或[2]之氧化鋁粉末，其中，前述被覆氧化鋁粒子中，球形度為0.80以下之被覆氧化鋁粒子的比例以個數基準計為15%以下。 [4] 如[1]～[3]中任一項之氧化鋁粉末，其中，利用雷射繞射散射式粒度分布測定儀測得的前述被覆氧化鋁粒子之平均粒徑為30μm以上150μm以下。 [5] 如[1]～[4]中任一項之氧化鋁粉末，其中，前述被覆氧化鋁粒子中之氮化鋁的含有率為10質量%以上40質量%以下。That is, the present invention is as follows. [1] An alumina powder containing coated alumina particles, The coated alumina particles have alumina particles and a coating layer that coats the aforementioned alumina particles, and the projected area circle equivalent diameter obtained by a microscope method is 1 μm or more and 300 μm or less; The aforementioned coating layer contains aluminum nitride; The average sphericity of the aforementioned coated alumina particles is 0.85 or more and 0.97 or less. [2] For example, the alumina powder of [1], wherein the volume-based frequency particle size distribution of the alumina powder obtained by the laser diffraction scattering method has multiple peaks in the particle size range of 2 μm to 200 μm. [3] The alumina powder of [1] or [2], wherein the proportion of the coated alumina particles having a sphericity of 0.80 or less among the coated alumina particles is 15% or less on a number basis. [4] The alumina powder of any one of [1] to [3], wherein the average particle size of the coated alumina particles measured by a laser diffraction scattering particle size distribution analyzer is 30 μm or more and 150 μm or less. [5] The alumina powder according to any one of [1] to [4], wherein the content of aluminum nitride in the coated alumina particles is 10% by mass or more and 40% by mass or less.

[6] 如[1]～[5]中任一項之氧化鋁粉末，其中，前述氧化鋁粉末中之氧化鋁與氮化鋁之合計含有率為80質量%以上。 [7] 如[1]～[6]中任一項之氧化鋁粉末，其中，前述被覆氧化鋁粒子中之碳量為0.3質量%以下。 [8] 一種樹脂組成物，含有樹脂、及如[1]～[7]中之任一項之氧化鋁粉末。 [9] 如[8]之樹脂組成物，其中，前述樹脂含有選自由聚矽氧樹脂、環氧樹脂、胺甲酸酯樹脂、及丙烯酸樹脂構成之群組中之至少1種。[6] The alumina powder of any one of [1] to [5], wherein the total content of alumina and aluminum nitride in the alumina powder is 80% by mass or more. [7] The alumina powder of any one of [1] to [6], wherein the amount of carbon in the coated alumina particles is 0.3% by mass or less. [8] A resin composition containing resin and alumina powder as in any one of [1] to [7]. [9] The resin composition of [8], wherein the aforementioned resin contains at least one selected from the group consisting of silicone resin, epoxy resin, urethane resin, and acrylic resin.

[10] 一種散熱零件，含有如[1]～[7]中任一項之氧化鋁粉末、或如[8]或[9]之樹脂組成物。 [11] 一種如[1]之被覆氧化鋁粉末之製造方法，包含下列步驟： 第1步驟，將含有原料之氧化鋁粉末與碳粉末的混合物於含有氮氣之還原氣氛下在1500℃以上1700℃以下之溫度進行煅燒，而獲得第1煅燒粉末；及 第2步驟，將前述第1煅燒粉末於大氣氣氛下在600℃以上900℃以下之溫度進一步煅燒，而獲得前述被覆氧化鋁粒子； 前述碳粉末之平均粒徑為30nm以上70nm以下，體密度(bulk density)為0.10g/cm3 以上0.20g/cm3 以下，比表面積為20m2 /g以上60m2 /g以下。 [發明之效果][10] A heat-dissipating component containing alumina powder as in any one of [1] to [7], or a resin composition as in [8] or [9]. [11] A method for manufacturing coated alumina powder as in [1], including the following steps: The first step is to put a mixture of alumina powder and carbon powder containing raw materials in a reducing atmosphere containing nitrogen at a temperature above 1500°C for 1700 Calcining at a temperature below °C to obtain the first calcined powder; and in the second step, the first calcined powder is further calcined in an air atmosphere at a temperature of 600°C or more and 900°C or less to obtain the coated alumina particles; The average particle diameter of the carbon powder is 30 nm or more and 70 nm or less, the bulk density is 0.10 g/cm 3 or more and 0.20 g/cm 3 or less, and the specific surface area is 20 m 2 /g or more and 60 m 2 /g or less. [Effects of Invention]

根據本發明，能提供填充於樹脂時可抑制黏度上升，且可達成含有該樹脂之樹脂組成物的高熱傳導化的氧化鋁粉末；並提供含有該氧化鋁粉末之樹脂組成物、散熱零件、及被覆氧化鋁粒子之製造方法。According to the present invention, it is possible to provide alumina powder that can suppress the increase in viscosity when filled with resin, and can achieve high thermal conductivity of the resin composition containing the resin; and provide the resin composition, heat dissipation parts, and the resin composition containing the alumina powder. Manufacturing method of coated alumina particles.

以下，針對用以實施本發明之形態(以下，簡稱為「本實施形態」。)進行詳細說明。此外，以下之本實施形態係用以說明本發明之例示，本發明不限定於本實施形態。Hereinafter, a mode for implementing the present invention (hereinafter, simply referred to as "this embodiment") will be described in detail. In addition, the following embodiment is an example for explaining the present invention, and the present invention is not limited to this embodiment.

[氧化鋁粉末] 本實施形態之氧化鋁粉末含有1種或2種以上之後述本實施形態之被覆氧化鋁粒子。本實施形態之氧化鋁粉末，如後述，亦可含有上述被覆氧化鋁粒子以外的填料，尤其可含有無機填料。本實施形態之氧化鋁粉末含有係上述被覆氧化鋁粒子以外的填料之無機填料以外的填料時，應單稱為粉末而不是稱為氧化鋁粉末。又，本實施形態之氧化鋁粉末含有上述被覆氧化鋁粒子以外的無機填料時(惟，不含無機填料以外的填料。)，應稱為無機粉末。惟，本說明書中，「氧化鋁粉末」係以包含該等之概念而使用。[Alumina powder] The alumina powder of this embodiment contains one kind or two or more kinds of coated alumina particles of this embodiment described later. The alumina powder of this embodiment may contain fillers other than the above-mentioned coated alumina particles, as described later, and may particularly contain an inorganic filler. When the alumina powder of the present embodiment contains fillers other than inorganic fillers other than the above-mentioned coated alumina particles, it should be referred to solely as powder instead of alumina powder. In addition, when the alumina powder of the present embodiment contains inorganic fillers other than the above-mentioned coated alumina particles (but does not contain fillers other than inorganic fillers), it should be referred to as an inorganic powder. However, in this manual, "alumina powder" is used to include these concepts.

(被覆氧化鋁粒子) 本實施形態之被覆氧化鋁粒子具有氧化鋁粒子、及將該氧化鋁粒子予以被覆且含有氮化鋁之被覆層，利用顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下，平均球形度為0.85以上0.97以下。以下，除非另有說明，否則亦將本實施形態之被覆氧化鋁粒子簡稱為「被覆氧化鋁粒子」。(Coated alumina particles) The coated alumina particles of this embodiment have alumina particles and a coating layer containing aluminum nitride to coat the alumina particles. The projected area obtained by the microscope method has a circle equivalent diameter of 1 μm or more and 300 μm or less, and the average sphericity is Above 0.85 and below 0.97. Hereinafter, unless otherwise stated, the coated alumina particles of this embodiment are also referred to simply as "coated alumina particles".

被覆氧化鋁粒子來自後述原料之氧化鋁粉末(以下，簡稱為「原料氧化鋁粉末」。)中含有的氧化鋁粒子。The coated alumina particles are derived from alumina particles contained in alumina powder (hereinafter referred to simply as "raw alumina powder") of the raw material described later.

藉由將含有被覆層含氮化鋁之被覆氧化鋁粒子的本實施形態之氧化鋁粉末使用於樹脂組成物及散熱零件，和後述使平均球形度成為預定數值範圍相互作用，樹脂組成物及散熱零件之熱傳導性尤其會提升。此外，被覆層亦可含有在形成被覆層之過程中產生的氮氧化鋁等不可避免的成分。By using the alumina powder of the present embodiment containing coated alumina particles containing aluminum nitride in the coating layer in the resin composition and heat dissipation parts, the resin composition and heat dissipation interact with each other to make the average sphericity into a predetermined numerical range as described later. The thermal conductivity of the parts is especially improved. In addition, the coating layer may contain inevitable components such as aluminum oxynitride generated in the process of forming the coating layer.

本實施形態之被覆層的厚度宜為0.8μm以上12μm以下，為1.5μm以上7.5μm以下的話，填充於樹脂時可適當地抑制黏度上升，或更可達成含有該樹脂之樹脂組成物的高熱傳導化，故更佳。使用被覆氧化鋁粒子中之被覆層之厚度為上述範圍內的氧化鋁粉末的話，有可有效率地形成熱路徑，能充分地傳導熱的傾向。被覆層的厚度係利用實施例記載之方法測定。The thickness of the coating layer of this embodiment is preferably 0.8 μm or more and 12 μm or less. If it is 1.5 μm or more and 7.5 μm or less, the increase in viscosity can be appropriately suppressed when filled with resin, or high thermal conductivity of the resin composition containing the resin can be achieved. So it’s better. If the alumina powder in which the thickness of the coating layer in the coated alumina particles falls within the above-mentioned range is used, there is a tendency that a heat path can be formed efficiently and heat can be sufficiently conducted. The thickness of the coating layer was measured by the method described in the examples.

本實施形態之被覆氧化鋁粒子，利用下列顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下，平均球形度為0.85以上0.97以下。被覆氧化鋁粒子之平均球形度為如上述範圍之球狀的話，將被覆氧化鋁粒子填充於樹脂時不易增黏。藉由本實施形態之氧化鋁粉末含有該被覆氧化鋁粒子，能將氧化鋁粉末以高比例填充於樹脂。其結果，樹脂中能以良好效率形成熱路徑，可獲得高熱傳導性之樹脂組成物及散熱零件。就該平均球形度而言，考量填充於樹脂時之摩擦阻力降低、及粒子彼此之接觸面積增加的觀點，宜為0.87以上0.96以下，為0.89以上0.95以下更佳。藉由本實施形態之氧化鋁粉末含有具有落在上述範圍之上述平均球形度的被覆氧化鋁粒子，樹脂中含有被覆氧化鋁粒子之氧化鋁粉末的流動性更為改善，與樹脂之摩擦阻力降低，可抑制將氧化鋁粉末填充於樹脂時的黏度上升。又，含有被覆氧化鋁粒子之氧化鋁粒子彼此的接觸更為充分，接觸面積變大，結果能以良好效率形成熱路徑，故有可獲得更高熱傳導性之樹脂組成物及散熱零件的傾向。平均球形度例如利用下列顯微鏡法測定。亦即，將利用掃描式電子顯微鏡、及穿透式電子顯微鏡等拍攝之粒子圖像讀入圖像解析裝置，由照片測定粒子之投影面積(A)與周圍長(PM)。令具有與該周圍長(PM)相同之周圍長的真圓之面積為(B)的話，該粒子之球形度為A/B。因此，假想具有與試樣之周圍長(PM)相同之周圍長的真圓的話，由於PM=2πr、B=πr2 ，故B=π×(PM/2π)2 ，各粒子之球形度為球形度=A/B=A×4π/(PM)2 。如上述般求出投影面積圓相當徑為1μm以上300μm以下之200個任意粒子的球形度，將其相加平均值定義為平均球形度。此外，具體的測定方法如實施例記載。又，投影面積圓相當徑係指具有與粒子之投影面積(A)相同之投影面積的真圓之直徑。The coated alumina particles of this embodiment have a projected area circle equivalent diameter obtained by the following microscope method of 1 μm or more and 300 μm or less, and an average sphericity of 0.85 or more and 0.97 or less. If the average sphericity of the coated alumina particles is spherical in the above-mentioned range, it is difficult to increase the viscosity when the coated alumina particles are filled in the resin. Since the alumina powder of this embodiment contains the coated alumina particles, the alumina powder can be filled in the resin at a high ratio. As a result, a heat path can be formed in the resin with good efficiency, and a resin composition and heat dissipation components with high thermal conductivity can be obtained. The average sphericity is preferably 0.87 or more and 0.96 or less, and more preferably 0.89 or more and 0.95 or less from the viewpoint of reducing frictional resistance when filled with resin and increasing the contact area between particles. Since the alumina powder of this embodiment contains the coated alumina particles having the above-mentioned average sphericity falling within the above range, the flowability of the alumina powder containing the coated alumina particles in the resin is improved, and the frictional resistance with the resin is reduced. The increase in viscosity when the alumina powder is filled in the resin can be suppressed. In addition, the alumina particles containing the coated alumina particles are in contact with each other more fully and the contact area becomes larger. As a result, a heat path can be formed with good efficiency, so there is a tendency to obtain a resin composition and a heat dissipation component with higher thermal conductivity. The average sphericity is measured by the following microscope method, for example. That is, the particle images taken by a scanning electron microscope, a transmission electron microscope, etc. are read into an image analysis device, and the projected area (A) and peripheral length (PM) of the particles are measured from the photos. If the area of a true circle having the same peripheral length (PM) as the peripheral length (PM) is (B), the sphericity of the particle is A/B. Therefore, assuming a true circle with the same peripheral length (PM) as the sample, since PM=2πr, B=πr 2 , so B=π×(PM/2π) 2 , the sphericity of each particle is Sphericity=A/B=A×4π/(PM) 2 . The sphericity of 200 arbitrary particles whose projected area circle equivalent diameter is 1 μm or more and 300 μm or less is obtained as described above, and the average value of the addition is defined as the average sphericity. In addition, the specific measurement method is as described in the Examples. In addition, the equivalent diameter of the projected area circle refers to the diameter of a true circle having the same projected area as the projected area (A) of the particle.

就本實施形態之氧化鋁粉末而言，本實施形態之被覆氧化鋁粒子中，球形度為0.80以下之被覆氧化鋁粒子的比例，以個數基準計宜為15%以下，以個數基準計為10%以下更佳。球形度為0.80以下之被覆氧化鋁粒子的比例以個數基準計為15%以下，意指係含有將氧化鋁粉末填充於樹脂時引起增黏之聚結粒子、破裂粒子少的被覆氧化鋁粒子之氧化鋁粉末，就此點而言係較佳。又，有可減低裝置及模具之磨耗的傾向。該被覆氧化鋁粒子的比例，例如以個數基準計為0.5%以上。又，利用顯微鏡法獲得之投影面積圓相當徑通常為200μm以下。Regarding the alumina powder of this embodiment, in the coated alumina particles of this embodiment, the proportion of coated alumina particles having a sphericity of 0.80 or less is preferably 15% or less on the basis of the number. It is more preferably 10% or less. The proportion of coated alumina particles with a sphericity of 0.80 or less is 15% or less based on the number, which means that it contains coalesced particles that cause adhesion when the alumina powder is filled in the resin, and the coated alumina particles with few broken particles The alumina powder is better in this regard. In addition, there is a tendency to reduce the wear of the device and the mold. The ratio of the coated alumina particles is, for example, 0.5% or more based on the number. In addition, the equivalent diameter of the circle of projected area obtained by the microscope method is usually 200 μm or less.

就本實施形態之氧化鋁粉末而言，本實施形態之被覆氧化鋁粒子中，球形度超過0.80且在0.83以下之被覆氧化鋁粒子的比例，以個數基準計宜為10%以下，以個數基準計為5%以下更佳。球形度為上述範圍之被覆氧化鋁粒子的比例為10%以下，意指係含有將氧化鋁粉末填充於樹脂時引起增黏之聚結粒子、破裂粒子較少的被覆氧化鋁粒子之氧化鋁粉末，就此點而言係較佳。又，有可減低裝置及模具之磨耗的傾向。該被覆氧化鋁粒子的比例，例如以個數基準計為0.5%以上。又，利用顯微鏡法獲得之投影面積圓相當徑通常為200μm以下。Regarding the alumina powder of this embodiment, in the coated alumina particles of this embodiment, the proportion of coated alumina particles with a sphericity exceeding 0.80 and below 0.83 is preferably 10% or less based on the number. It is better to count as 5% or less on a numerical basis. The proportion of the coated alumina particles with the sphericity in the above range is 10% or less, which means that the alumina powder contains agglomerated particles that cause adhesion when the alumina powder is filled in the resin, and the alumina powder of the coated alumina particles with fewer broken particles , In this regard is better. In addition, there is a tendency to reduce the wear of the device and the mold. The ratio of the coated alumina particles is, for example, 0.5% or more based on the number. In addition, the equivalent diameter of the circle of projected area obtained by the microscope method is usually 200 μm or less.

本實施形態之被覆氧化鋁粒子，含有被覆氧化鋁粒子之氧化鋁粉末彼此的接觸變得更良好，有能以良好效率形成熱路徑，可獲得更高熱傳導性之樹脂組成物及散熱零件的傾向，進一步考量製成樹脂組成物時之表面平滑性的觀點，平均粒徑宜為30μm以上150μm以下，為30μm以上130μm以下更佳，為40μm以上120μm以下又更佳。平均粒徑為30μm以上的話，有在樹脂組成物及散熱零件中可更有效率地形成熱路徑，能更充分地傳導熱的傾向。又，平均粒徑為150μm以下的話，散熱零件之表面的平滑性進一步得到改善，於散熱零件與熱源之界面的熱阻減小，故有可更充分地改善熱傳導率的傾向。此外，本實施形態中，粒徑及平均粒徑係利用雷射繞射散射式粒度分布測定儀測定。具體的測定方法如實施例記載。In the coated alumina particles of this embodiment, the contact between the alumina powders containing the coated alumina particles becomes better, the heat path can be formed with good efficiency, and the resin composition and heat dissipating parts with higher thermal conductivity tend to be obtained. In consideration of the surface smoothness of the resin composition, the average particle size is preferably 30 μm or more and 150 μm or less, more preferably 30 μm or more and 130 μm or less, and more preferably 40 μm or more and 120 μm or less. If the average particle size is 30 μm or more, there is a tendency that a heat path can be formed more efficiently in the resin composition and heat dissipation parts, and heat can be conducted more fully. In addition, when the average particle size is 150 μm or less, the smoothness of the surface of the heat dissipation component is further improved, and the thermal resistance at the interface between the heat dissipation component and the heat source is reduced, so there is a tendency that the thermal conductivity can be more fully improved. In addition, in this embodiment, the particle size and the average particle size are measured by a laser diffraction scattering type particle size distribution analyzer. The specific measurement method is as described in the examples.

本實施形態之被覆氧化鋁粒子中之氮化鋁的含有率，宜為10質量%以上40質量%以下，為了進一步達成樹脂組成物的高熱傳導化，為15質量%以上35質量%以下更佳。使用氮化鋁之含有率為上述範圍內的被覆氧化鋁粒子的話，有可更有效率地形成熱路徑，能更充分地傳導熱的傾向。該含有率為10質量%以上的話，氮化鋁之被覆層變得更厚，故有因被覆有氮化鋁所獲致之熱導電率改善的效果進一步提升的傾向。該含有率為40質量%以下的話，可更減少被覆層之微小凹凸，故有樹脂組成物及散熱零件的成形性更為改善，可進一步減少散熱零件中的空隙的傾向。氮化鋁的含有率係利用實施例記載之方法測定。The content of aluminum nitride in the coated alumina particles of this embodiment is preferably 10% by mass or more and 40% by mass or less. In order to further achieve high thermal conductivity of the resin composition, it is more preferably 15% by mass or more and 35% by mass or less. . If the coated alumina particles having the aluminum nitride content within the above range are used, there is a tendency that a heat path can be formed more efficiently, and heat can be conducted more fully. When the content is 10% by mass or more, the coating layer of aluminum nitride becomes thicker, and therefore, the effect of improving the thermal conductivity due to the coating with aluminum nitride tends to be further enhanced. If the content is 40% by mass or less, the microscopic unevenness of the coating layer can be reduced, so the moldability of the resin composition and the heat dissipating part is improved, and the tendency of voids in the heat dissipating part can be further reduced. The content of aluminum nitride was measured by the method described in the examples.

本實施形態之被覆氧化鋁粒子中之碳量，宜為0.3質量%以下，為0.2質量%以下更佳，為0.1質量%以下又更佳。又，該被覆氧化鋁粒子中之碳量，例如為0.01質量%以上。藉由碳量為上述範圍，有具有更良好之熱傳導性的傾向，由於盡可能地減少作為導電物之碳，可更有效且確實地獲得具有高絕緣性、及熱傳導率的樹脂組成物及散熱零件。被覆氧化鋁粒子中之碳量係利用實施例記載之方法測定。又，被覆氧化鋁粒子中之碳主要來自與原料氧化鋁粉末混合之碳粉末。碳粉末如在後述被覆氧化鋁粒子之製造方法中所說明，係於製造本實施形態之被覆氧化鋁粒子時使用。The amount of carbon in the coated alumina particles of this embodiment is preferably 0.3% by mass or less, more preferably 0.2% by mass or less, and even more preferably 0.1% by mass or less. In addition, the amount of carbon in the coated alumina particles is, for example, 0.01% by mass or more. When the amount of carbon is in the above range, there is a tendency to have better thermal conductivity. Since carbon as a conductive material is reduced as much as possible, a resin composition with high insulation and thermal conductivity and heat dissipation can be obtained more effectively and reliably. Components. The amount of carbon in the coated alumina particles was measured by the method described in the examples. In addition, the carbon in the coated alumina particles mainly comes from carbon powder mixed with raw alumina powder. The carbon powder is used when manufacturing the coated alumina particles of the present embodiment, as explained in the method of manufacturing the coated alumina particles described later.

本實施形態之被覆氧化鋁粒子的比表面積，宜為0.02m2 /g以上0.15m2 /g以下，為0.03m2 /g以上0.12m2 /g以下更佳。比表面積為上述範圍的話，可發揮容易抑制將含有特定被覆氧化鋁粒子之氧化鋁粉末填充於樹脂時之黏度上升，而能獲得更高熱傳導性之樹脂組成物及散熱零件的效果。此外，本實施形態中，比表面積係利用BET流動法測定，具體的測定方法如實施例記載。The specific surface area of the present embodiment forms coated alumina particles, is suitably 0.02m 2 / g or more 0.15m 2 / g or less, was 0.03m 2 / g or more 0.12m 2 / g or less more preferably. When the specific surface area is in the above range, it is possible to easily suppress the increase in viscosity when the alumina powder containing the specific coated alumina particles is filled in the resin, and to obtain a resin composition and heat dissipation parts with higher thermal conductivity. In addition, in this embodiment, the specific surface area is measured by the BET flow method, and the specific measurement method is as described in the examples.

(氧化鋁粉末) 本實施形態之氧化鋁粉末中，氧化鋁與氮化鋁之合計含有率，宜為80質量%以上，為85質量%以上更佳，為90質量%以上又更佳，為99質量%以上尤佳。該合計含有率的上限例如為100質量%。氧化鋁與氮化鋁之合計含有率為上述範圍內的氧化鋁粉末，由於有妨礙熱路徑之傾向的氮氧化鋁等不可避免的成分變得更少，故有可獲得更高熱傳導性之樹脂組成物及散熱零件的傾向。氧化鋁與氮化鋁之合計含有率係利用實施例記載之方法測定。(Alumina powder) In the alumina powder of this embodiment, the total content of alumina and aluminum nitride is preferably 80% by mass or more, more preferably 85% by mass or more, more preferably 90% by mass or more, and particularly 99% by mass or more good. The upper limit of the total content rate is, for example, 100% by mass. Alumina powder with the total content of alumina and aluminum nitride within the above-mentioned range has fewer unavoidable components such as aluminum oxynitride, which tend to obstruct the heat path. Therefore, there are resins that can achieve higher thermal conductivity. The tendency of the composition and heat-dissipating parts. The total content of alumina and aluminum nitride was measured by the method described in the examples.

就本實施形態之氧化鋁粉末而言，利用雷射繞射散射法獲得之體積基準頻率粒度分布中，宜於粒徑為2μm以上200μm以下之粒度範圍具有多個峰部。藉此，本實施形態之氧化鋁粉末能以良好效率填充於樹脂，從而可形成熱路徑，並可達成高熱傳導化，而且樹脂組成物的黏度上升得到抑制。此處，本實施形態中，峰部係指在利用雷射繞射散射法獲得之體積基準頻率粒度分布中，將0.01μm以上3500μm以下之粒徑範圍分割成100區段，於該粒徑範圍檢測到的極大點。又，檢測到的峰部中有肩部時，該肩部亦計數為峰部。肩部，意指以由二次微分係數導出之峰部的曲率檢測，於峰部中具有反曲點，亦即，存在更多特定粒徑之粒子成分。For the alumina powder of this embodiment, in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method, it is preferable that the particle size range of 2 μm or more and 200 μm or less has multiple peaks. As a result, the alumina powder of the present embodiment can be efficiently filled in the resin, thereby forming a heat path, achieving high thermal conductivity, and suppressing the increase in the viscosity of the resin composition. Here, in this embodiment, the peak part means that the particle size range of 0.01 μm or more and 3500 μm or less is divided into 100 segments in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method. The maximum point detected. In addition, when there is a shoulder in the detected peak, the shoulder is also counted as a peak. The shoulder part means to detect the curvature of the peak part derived from the second differential coefficient. There is an inflection point in the peak part, that is, there are more particle components of a specific particle size.

就本實施形態之氧化鋁粉末而言，利用雷射繞射散射法獲得之體積基準頻率粒度分布中，於粒徑為0.01μm以上3500μm以下之粒度範圍具有1個以上之來自被覆氧化鋁粒子的峰部。本實施形態之氧化鋁粉末，亦可在利用雷射繞射散射法獲得之體積基準頻率粒度分布中，於粒徑為0.01μm以上3500μm以下之粒度範圍具有多個來自本實施形態之被覆氧化鋁粒子的峰部。With regard to the alumina powder of this embodiment, in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method, there are more than 1 particles derived from the coated alumina particles in the particle size range of 0.01 μm or more and 3500 μm or less. Peak. The alumina powder of this embodiment can also have multiple coated aluminas from this embodiment in the particle size range of 0.01 μm to 3500 μm in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method. The peak of the particle.

具有如此之粒度分布的氧化鋁粉末，例如可藉由含有分別於上述粒度範圍具有1個峰部且平均粒徑彼此不同的2種以上之被覆氧化鋁粒子而獲得。The alumina powder having such a particle size distribution can be obtained, for example, by containing two or more kinds of coated alumina particles each having one peak in the above-mentioned particle size range and having different average particle sizes from each other.

另外，本實施形態之氧化鋁粉末中亦可含有本實施形態之被覆氧化鋁粒子以外的填料。即使在該情形下，通常也會在利用雷射繞射散射法獲得之體積基準頻率粒度分布中，於粒徑為0.01μm以上3500μm以下之粒度範圍檢測到來自本實施形態之被覆氧化鋁粒子的峰部、與來自該被覆氧化鋁粒子以外的填料的峰部之2個以上之峰部。就填料而言，例如可列舉無機填料。具體而言，可列舉本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子、不具有被覆層的(亦即，未被覆的)氧化鋁粒子、氧化鎂、氮化鋁、氮化矽、氧化釔、氮化硼、氧化鈣、氧化鐵、及氧化硼。此外，本實施形態之氧化鋁粉末，如上述亦含有以氮化鋁為首的氧化鋁以外的無機材料，就此點而言，相當於無機粉末。In addition, the alumina powder of this embodiment may contain fillers other than the coated alumina particles of this embodiment. Even in this case, in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method, the particles from the coated alumina particles of this embodiment are usually detected in the particle size range of 0.01 μm to 3500 μm. Two or more peaks among peaks and peaks derived from fillers other than the coated alumina particles. As for the filler, for example, an inorganic filler can be cited. Specifically, coated alumina particles other than the coated alumina particles of the present embodiment, alumina particles without a coating layer (that is, uncoated), magnesium oxide, aluminum nitride, silicon nitride, oxide Yttrium, boron nitride, calcium oxide, iron oxide, and boron oxide. In addition, the alumina powder of the present embodiment also contains inorganic materials other than alumina such as aluminum nitride as described above, and in this regard, it corresponds to an inorganic powder.

被覆氧化鋁粒子以外的被覆氧化鋁粒子，例如可列舉具有氧化鋁粒子、與將該氧化鋁粒子予以被覆之被覆層，且利用顯微鏡法獲得之投影面積圓相當徑未達1μm的被覆氧化鋁粒子。此時的被覆層，例如可列舉氮化鋁、及氮化矽。Coated alumina particles other than coated alumina particles include, for example, coated alumina particles having alumina particles and a coating layer covering the alumina particles, and having a projected area circle equivalent diameter of less than 1 μm obtained by a microscope method . Examples of the coating layer at this time include aluminum nitride and silicon nitride.

又，本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子，可列舉係具有氧化鋁粒子、與將該氧化鋁粒子予以被覆之被覆層，且利用顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下的被覆氧化鋁粒子，且係被覆層不含氮化鋁的被覆氧化鋁粒子。此時的被覆層，例如可列舉氮化矽。In addition, the coated alumina particles other than the coated alumina particles of the present embodiment include alumina particles and a coating layer that coats the alumina particles, and the projected area circle equivalent diameter obtained by the microscope method is 1 μm. The above-mentioned coated alumina particles of 300 μm or less are coated alumina particles whose coating layer does not contain aluminum nitride. For the coating layer at this time, for example, silicon nitride can be cited.

該等填料亦可為經使用公知的矽烷偶聯劑等進行表面處理的填料。 本實施形態之氧化鋁粉末中，可與本實施形態之被覆氧化鋁粒子一起含有1種或2種以上之該等填料。These fillers may also be those that have been surface-treated using a well-known silane coupling agent or the like. The alumina powder of this embodiment may contain one or more of these fillers together with the coated alumina particles of this embodiment.

本實施形態之氧化鋁粉末中，相對於該氧化鋁粉末之總量，本實施形態之被覆氧化鋁粒子之含量宜為20體積%以上80體積%以下，為25體積%以上75體積%以下更佳。此外，本實施形態中，氧化鋁粉末中含有平均粒徑彼此不同的2種以上之本實施形態之被覆氧化鋁粒子時，該被覆氧化鋁粒子之含量為它們的合計量。藉由於上述範圍內含有被覆氧化鋁粒子，本實施形態之氧化鋁粉末在填充於樹脂時可進一步抑制黏度上升，且更可達成含有該樹脂之樹脂組成物的高熱傳導化。In the alumina powder of this embodiment, relative to the total amount of the alumina powder, the content of the coated alumina particles of this embodiment is preferably 20% by volume to 80% by volume, and more preferably 25% by volume to 75% by volume. good. In addition, in this embodiment, when the alumina powder contains two or more kinds of coated alumina particles of this embodiment having different average particle sizes from each other, the content of the coated alumina particles is the total amount thereof. Since the coated alumina particles are contained within the above-mentioned range, the alumina powder of the present embodiment can further suppress the increase in viscosity when it is filled in the resin, and can further achieve high thermal conductivity of the resin composition containing the resin.

又，本實施形態之氧化鋁粉末中，考量改善熱傳導率的觀點，相對於該氧化鋁粉末之總量，本實施形態之被覆氧化鋁粒子、本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子、及未被覆的氧化鋁粒子(以下，稱為「被覆氧化鋁粒子等」。)之合計含量宜為80體積%以上100體積%以下，為85體積%以上100體積%以下更佳。藉由於上述範圍內含有被覆氧化鋁粒子等，本實施形態之氧化鋁粉末具有樹脂組成物之高熱傳導化的效果。In addition, in the alumina powder of this embodiment, considering the viewpoint of improving the thermal conductivity, the coated alumina particles of this embodiment and the coated alumina other than the coated alumina particles of this embodiment are relative to the total amount of the alumina powder. The total content of particles and uncoated alumina particles (hereinafter referred to as "coated alumina particles, etc.") is preferably 80% by volume to 100% by volume, and more preferably 85% by volume to 100% by volume. Since the coated alumina particles and the like are contained within the above-mentioned range, the alumina powder of the present embodiment has the effect of increasing the thermal conductivity of the resin composition.

本實施形態之氧化鋁粉末，於粒徑為2μm以上200μm以下之粒度範圍，如上述宜具有多個峰部，亦即具有2個以上之峰部較佳，具有2個以上4個以下之峰部更佳，具有3個峰部又更佳。此外，針對各峰部，在利用雷射繞射散射法獲得之體積基準頻率粒度分布中，自粒徑為0.01μm以上3500μm以下之粒度範圍之微粒側(亦即，0.01μm側)，將具有檢測到之第1個峰部的粒子定義為第1粒子，具有第2個峰部之粒子定義為第2粒子，按照順序具有第n個峰部之粒子定義為第n粒子。亦即，檢測到之峰部數為n。檢測到之粒子可僅為本實施形態之被覆氧化鋁粒子，也可除此之外為該被覆氧化鋁粒子以外的填料，但本實施形態之被覆氧化鋁粒子以外的填料宜為本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子及未被覆的氧化鋁粒子中之1種以上。The alumina powder of this embodiment has a particle size range of 2μm or more and 200μm or less, as mentioned above, it is better to have multiple peaks, that is, it is better to have 2 or more peaks, and 2 or more and 4 or less peaks. The part is better, and it is even better to have 3 peaks. In addition, for each peak portion, in the volume-based frequency particle size distribution obtained by the laser diffraction scattering method, the particle size from the particle size range of 0.01 μm to 3500 μm (that is, the 0.01 μm side) will have The detected particle with the first peak is defined as the first particle, the particle with the second peak is defined as the second particle, and the particle with the n-th peak in order is defined as the n-th particle. That is, the number of peaks detected is n. The detected particles may be only the coated alumina particles of this embodiment, or fillers other than the coated alumina particles. However, fillers other than the coated alumina particles of this embodiment are preferably the coated alumina particles of this embodiment One or more of coated alumina particles other than alumina particles and uncoated alumina particles.

本實施形態之氧化鋁粉末，當峰部數n為2時，宜為來自第1粒子之峰部的位置於3μm以上15μm以下之粒度範圍被檢測到，來自第2粒子之峰部的位置於30μm以上150μm以下之粒度範圍被檢測到較佳。又，第2粒子宜為本實施形態之被覆氧化鋁粒子，除此之外第1粒子為未被覆的氧化鋁粒子更佳。 本實施形態之氧化鋁粉末中之第1粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為25體積%以上55體積%以下，宜為30體積%以上50體積%以下，為35體積%以上45體積%以下更佳。第2粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為45體積%以上75體積%以下，宜為50體積%以上70體積%以下，為55體積%以上65體積%以下更佳。此外，第1粒子與第2粒子之合計為100體積%。 又，第1粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為4.0μm以上12μm以下，為5.0μm以上10μm以下更佳。第2粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為35μm以上140μm以下，為40μm以上130μm以下更佳。For the alumina powder of this embodiment, when the number of peaks n is 2, it is preferable that the peak position from the first particle is detected in the particle size range of 3 μm to 15 μm, and the peak position from the second particle is The particle size range of 30 μm or more and 150 μm or less is better detected. In addition, the second particles are preferably coated alumina particles of this embodiment, except that the first particles are more preferably uncoated alumina particles. The content of the first particles in the alumina powder of this embodiment, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 25% by volume to 55% by volume, preferably 30% by volume to 50% by volume, and 35 It is more preferably not less than vol% and not more than 45 vol%. The content of the second particles, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 45% by volume to 75% by volume, preferably from 50% by volume to 70% by volume, and more preferably from 55% by volume to 65% by volume. . In addition, the total of the first particles and the second particles is 100% by volume. In addition, the average particle diameter of the first particles is preferably 4.0 μm or more and 12 μm or less, and more preferably 5.0 μm or more and 10 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition. The average particle diameter of the second particles is preferably 35 μm or more and 140 μm or less, and more preferably 40 μm or more and 130 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition.

峰部數n為3時，宜為來自第1粒子之峰部的位置於0.3μm以上1.0μm以下之粒度範圍被檢測到，來自第2粒子之峰部的位置於3.0μm以上15μm以下之粒度範圍被檢測到，來自第3粒子之峰部的位置於30μm以上150μm以下之粒度範圍被檢測到較佳。 本實施形態之氧化鋁粉末中之第1粒子的含有率，為10體積%以上25體積%以下，宜為12體積%以上18體積%以下，為13體積%以上17體積%以下更佳。又，第2粒子的含有率為20體積%以上55體積%以下，宜為25體積%以上41體積%以下，為30體積%以上39體積%以下更佳。另外，第3粒子的含有率為35體積%以上55體積%以下，宜為47體積%以上57體積%以下，為48體積%以上53體積%以下更佳。各粒子的含有率落在上述範圍的話，可將氧化鋁粉末以高比例填充於樹脂，進一步考量抑制樹脂組成物之黏度上升的觀點係較佳。此外，第1粒子、第2粒子、及第3粒子之合計為100體積%。When the number of peaks n is 3, it is suitable that the particle size range from the peak position of the first particle is between 0.3μm and 1.0μm, and the particle size range from the peak position of the second particle is 3.0μm to 15μm. The range is detected, and the particle size range from 30 μm to 150 μm from the position of the peak of the third particle is preferably detected. The content of the first particles in the alumina powder of this embodiment is 10% by volume or more and 25% by volume or less, preferably 12% by volume or more and 18% by volume or less, and more preferably 13% by volume or more and 17% by volume or less. In addition, the content of the second particles is 20 vol% or more and 55 vol% or less, preferably 25 vol% or more and 41 vol% or less, and more preferably 30 vol% or more and 39 vol% or less. In addition, the content of the third particles is 35 vol% or more and 55 vol% or less, preferably 47 vol% or more and 57 vol% or less, and more preferably 48 vol% or more and 53 vol% or less. If the content of each particle falls within the above-mentioned range, the alumina powder can be filled in the resin at a high ratio, and it is preferable from the viewpoint of suppressing the increase in the viscosity of the resin composition. In addition, the total of the first particles, the second particles, and the third particles is 100% by volume.

此時，第1粒子之平均粒徑宜為0.3μm以上1.0μm以下，為0.4μm以上0.9μm以下更佳，為0.5μm以上0.8μm以下又更佳。藉由第1粒子之平均粒徑為0.3μm以上，有能以良好效率填充粒子間之間隙，可改善熱傳導性，進一步可獲得抑制樹脂組成物之黏度上升的效果的傾向。又，藉由第1粒子之平均粒徑為1.0μm以下，相較於平均粒徑超過1.0μm之情形，第1粒子之含量為相同程度時，有粒子數變多，粒子間之熱路徑數亦增加的傾向。另一方面，平均粒徑超過1.0μm時，有粒子間之熱路徑數減少的傾向。又，平均粒徑超過1.0μm時，於第1粒子內之熱傳導雖快速，但於數目較少之熱路徑之熱傳導成為速率決定因素，就粉末整體觀之時熱傳導性有變低的傾向。但是，平均粒徑為1.0μm以下時，各粒子之粒徑小，且熱路徑數多，故於第1粒子內之熱傳導與於粒子間之熱路徑之熱傳導間不易產生大的差異，熱傳導的均勻性變高，結果有熱傳導性變高的傾向。In this case, the average particle diameter of the first particles is preferably 0.3 μm or more and 1.0 μm or less, more preferably 0.4 μm or more and 0.9 μm or less, and more preferably 0.5 μm or more and 0.8 μm or less. When the average particle diameter of the first particles is 0.3 μm or more, the gaps between the particles can be filled efficiently, the thermal conductivity can be improved, and the effect of suppressing the increase in the viscosity of the resin composition tends to be obtained. In addition, since the average particle size of the first particles is 1.0 μm or less, compared to the case where the average particle size exceeds 1.0 μm, when the content of the first particles is the same, the number of particles increases, and the number of heat paths between the particles Also increase the tendency. On the other hand, when the average particle size exceeds 1.0 μm, the number of heat paths between particles tends to decrease. In addition, when the average particle size exceeds 1.0 μm, the heat conduction in the first particles is rapid, but the heat conduction in a small number of heat paths becomes the speed determining factor, and the thermal conductivity tends to be lower in the overall view of the powder. However, when the average particle size is 1.0 μm or less, the particle size of each particle is small and the number of heat paths is large. Therefore, the heat conduction in the first particle and the heat conduction between the particles are not likely to have a big difference. As the uniformity becomes higher, the thermal conductivity tends to become higher as a result.

又，第2粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為3.0μm以上15μm以下，為4.0μm以上12μm以下更佳，為5.0μm以上10μm以下又更佳。藉由第2粒子之平均粒徑為上述範圍，有第2粒子能以良好效率填充粒子間之間隙，可改善熱傳導性，進一步可獲得抑制樹脂組成物之黏度上升的效果的傾向。In addition, the average particle diameter of the second particles is preferably 3.0 μm or more and 15 μm or less, more preferably 4.0 μm or more and 12 μm or less, and more preferably 5.0 μm or more and 10 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition. When the average particle size of the second particles is in the above range, the second particles can efficiently fill the gaps between the particles, improve thermal conductivity, and further obtain the effect of suppressing the increase in the viscosity of the resin composition.

第3粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為30μm以上140μm以下，為35μm以上135μm以下更佳，為45μm以上130μm以下又更佳，為60μm以上120μm以下尤佳。藉由第3粒子之平均粒徑為30μm以上，利用粒子彼此的接觸，可有效率地形成熱路徑，故有可改善熱傳導性的傾向。另外，粒子的比表面積變小，藉此，有可提高填充率的傾向。又，藉由第3粒子之平均粒徑為140μm以下，可保持獲得之散熱零件的表面平滑性，且可降低粒子界面之接觸阻力，故有可提高熱傳導性的傾向。The average particle size of the third particle is preferably 30 μm or more and 140 μm or less, more preferably 35 μm or more and 135 μm or less, more preferably 45 μm or more and 130 μm or less, and more preferably 60 μm or more and 120 μm or less from the viewpoint of suppressing the increase in viscosity of the resin composition. . Since the average particle diameter of the third particles is 30 μm or more, the contact between the particles can form a heat path efficiently, and therefore, there is a tendency that the thermal conductivity can be improved. In addition, the specific surface area of the particles becomes smaller, whereby the filling rate tends to be improved. In addition, since the average particle size of the third particles is 140 μm or less, the surface smoothness of the obtained heat dissipation component can be maintained, and the contact resistance of the particle interface can be reduced, so the thermal conductivity tends to be improved.

又，第1粒子之平均球形度，考量降低填充於樹脂時之摩擦阻力、及增加粒子彼此之接觸面積的觀點，宜為0.82以上0.94以下，為0.84以上0.92以下更佳。 第2粒子之平均球形度，考量降低填充於樹脂時之摩擦阻力、及增加粒子彼此之接觸面積的觀點，宜為0.82以上0.94以下，為0.84以上0.92以下更佳。 第3粒子之平均球形度，考量降低填充於樹脂時之摩擦阻力、及增加粒子彼此之接觸面積的觀點，宜為0.82以上0.94以下，為0.84以上0.92以下更佳。In addition, the average sphericity of the first particles is preferably 0.82 or more and 0.94 or less, and more preferably 0.84 or more and 0.92 or less from the viewpoint of reducing frictional resistance when filled with resin and increasing the contact area between particles. The average sphericity of the second particles is preferably 0.82 or more and 0.94 or less, and more preferably 0.84 or more and 0.92 or less, in consideration of reducing frictional resistance when filled with resin and increasing the contact area between particles. The average sphericity of the third particles is preferably 0.82 or more and 0.94 or less, and more preferably 0.84 or more and 0.92 or less from the viewpoint of reducing frictional resistance when filled with resin and increasing the contact area between particles.

第1粒子中之α結晶相的含有率，考量改善熱傳導率的觀點，宜為80質量%以上，為90質量%以上更佳。上限例如為100質量%。 第2粒子中之α結晶相的含有率，考量改善熱傳導率的觀點，宜為80質量%以上，為90質量%以上更佳。上限例如為100質量%。 第3粒子中之α結晶相的含有率，考量改善熱傳導率的觀點，宜為80質量%以上，為90質量%以上更佳。上限例如為100質量%。The content of the α crystal phase in the first particles is preferably 80% by mass or more, and more preferably 90% by mass or more, from the viewpoint of improving the thermal conductivity. The upper limit is, for example, 100% by mass. The content of the α crystal phase in the second particles is preferably 80% by mass or more, and more preferably 90% by mass or more, from the viewpoint of improving the thermal conductivity. The upper limit is, for example, 100% by mass. The content of the α crystal phase in the third particles is preferably 80% by mass or more, and more preferably 90% by mass or more, from the viewpoint of improving the thermal conductivity. The upper limit is, for example, 100% by mass.

本實施形態中，就第1粒子而言，考量進一步改善流動性的觀點，宜為未被覆的氧化鋁粒子。 就第2粒子而言，考量改善流動性、及熱傳導率的觀點，宜為未被覆的氧化鋁粒子、本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子、及本實施形態之被覆氧化鋁粒子，為未被覆的氧化鋁粒子更佳。 就第3粒子而言，考量改善熱傳導率的觀點，宜為本實施形態之被覆氧化鋁粒子、未被覆的氧化鋁粒子、及本實施形態之被覆氧化鋁粒子以外的被覆氧化鋁粒子，為本實施形態之被覆氧化鋁粒子更佳。 作為未被覆的氧化鋁粒子，例如可列舉球狀氧化鋁粒子。In this embodiment, the first particles are preferably uncoated alumina particles from the viewpoint of further improving fluidity. As for the second particles, from the viewpoints of improving fluidity and thermal conductivity, they are preferably uncoated alumina particles, coated alumina particles other than the coated alumina particles of this embodiment, and coated alumina of this embodiment The particles are preferably uncoated alumina particles. Regarding the third particle, from the viewpoint of improving the thermal conductivity, the coated alumina particles of this embodiment, the uncoated alumina particles, and the coated alumina particles other than the coated alumina particles of this embodiment are suitable. The coated alumina particles of the embodiment are more preferable. Examples of the uncoated alumina particles include spherical alumina particles.

峰部數n為4時，宜為來自第1粒子之峰部的位置於0.05μm以上0.2μm以下之粒度範圍被檢測到，來自第2粒子之峰部的位置於0.3μm以上1.0μm以下之粒度範圍被檢測到，來自第3粒子之峰部的位置於3.0μm以上15μm以下之粒度範圍被檢測到，來自第4粒子之峰部的位置於30μm以上150μm以下之粒度範圍被檢測到較佳。本實施形態之氧化鋁粉末，考量抑制樹脂組成物之黏度上升的觀點，來自第1粒子之峰部的位置於0.07μm以上0.1μm以下之粒度範圍被檢測到，來自第2粒子之峰部的位置於0.4μm以上0.9μm以下之粒度範圍被檢測到，來自第3粒子之峰部的位置於4.0μm以上12μm以下之粒度範圍被檢測到，來自第4粒子之峰部的位置於35μm以上140μm以下之粒度範圍被檢測到更佳。又，第4粒子宜為本實施形態之被覆氧化鋁粒子，除此之外第1粒子、第2粒子及第3粒子為未被覆的氧化鋁粒子更佳。When the number of peaks n is 4, it is preferable that the peak position from the first particle is detected within a particle size range of 0.05 μm to 0.2 μm, and the peak position from the second particle is within 0.3 μm to 1.0 μm. The particle size range is detected. The particle size range from the peak of the third particle is detected from 3.0μm to 15μm, and the particle size range from the peak of the fourth particle is detected from 30μm to 150μm. . In the alumina powder of this embodiment, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, the particle size range from the peak of the first particle to 0.07μm to 0.1μm is detected, and the particle size range from the peak of the second particle is detected. The particle size range from 0.4μm to 0.9μm is detected, the particle size range from the peak of the third particle is from 4.0μm to 12μm, and the particle size from the peak of the fourth particle is from 35μm to 140μm. The following particle size range is better detected. In addition, the fourth particle is preferably the coated alumina particle of this embodiment, and it is more preferable that the first particle, the second particle, and the third particle are uncoated alumina particles.

本實施形態之氧化鋁粉末中之第1粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為0.5體積%以上5.0體積%以下，宜為1.0體積%以上4.0體積%以下，為1.5體積%以上3.0體積%以下更佳。第2粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為9體積%以上20體積%以下，宜為11體積%以上18體積%以下，為12體積%以上17體積%以下更佳。第3粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為19體積%以上45體積%以下，宜為24體積%以上41體積%以下，為29體積%以上39體積%以下更佳。第4粒子的含有率，考量抑制樹脂組成物之黏度上升的觀點，為43體積%以上60體積%以下，宜為45體積%以上57體積%以下，為46體積%以上53體積%以下更佳。此外，第1粒子、第2粒子、第3粒子、第4粒子之合計為100體積%。The content of the first particles in the alumina powder of this embodiment, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 0.5 vol% to 5.0 vol%, preferably 1.0 vol% to 4.0 vol%, and 1.5 It is more preferably not less than vol% and not more than 3.0 vol%. The content of the second particles, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 9 vol% or more and 20 vol% or less, preferably 11 vol% or more and 18 vol% or less, and more preferably 12 vol% or more and 17 vol% or less . The content of the third particle, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 19 vol% to 45 vol%, preferably 24 vol% to 41 vol%, and more preferably 29 vol% to 39 vol%. . The content of the fourth particle, considering the viewpoint of suppressing the increase in the viscosity of the resin composition, is 43 vol% or more and 60 vol% or less, preferably 45 vol% or more and 57 vol% or less, and more preferably 46 vol% or more and 53 vol% or less . In addition, the total of the first particles, the second particles, the third particles, and the fourth particles is 100% by volume.

又，第1粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為0.05μm以上0.2μm以下，為0.07μm以上0.1μm以下更佳。第2粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為0.3μm以上1.0μm以下，為0.4μm以上0.9μm以下更佳。第3粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為3.0μm以上15μm以下，為4.0μm以上12μm以下更佳。第4粒子之平均粒徑，考量抑制樹脂組成物之黏度上升的觀點，宜為30μm以上150μm以下，為35μm以上140μm以下更佳。In addition, the average particle diameter of the first particles is preferably 0.05 μm or more and 0.2 μm or less, and more preferably 0.07 μm or more and 0.1 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition. The average particle diameter of the second particles is preferably 0.3 μm or more and 1.0 μm or less, and more preferably 0.4 μm or more and 0.9 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition. The average particle diameter of the third particles is preferably 3.0 μm or more and 15 μm or less, and more preferably 4.0 μm or more and 12 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition. The average particle size of the fourth particles is preferably 30 μm or more and 150 μm or less, and more preferably 35 μm or more and 140 μm or less from the viewpoint of suppressing the increase in the viscosity of the resin composition.

本實施形態中，氧化鋁粉末中之第1～第n粒子全部之合計含有率，考量改善熱傳導率的觀點，宜為98體積%以上，為99體積%以上更佳。此外，含有率的上限為100體積%。In the present embodiment, the total content of all the first to nth particles in the alumina powder is preferably 98 vol% or more, and more preferably 99 vol% or more from the viewpoint of improving the thermal conductivity. In addition, the upper limit of the content rate is 100% by volume.

(被覆氧化鋁粒子之製造方法) 就本實施形態之被覆氧化鋁粒子之製造方法而言，例如可藉由使用包含下列步驟之步驟獲得：第1步驟，將含有原料氧化鋁粉末與碳粉末的混合物於含有氮氣之還原氣氛下在1500℃以上1700℃以下之溫度進行煅燒，而獲得第1煅燒粉末；第2步驟，將第1煅燒粉末於大氣氣氛下在600℃以上900℃以下之溫度進一步煅燒，而獲得本實施形態之被覆氧化鋁粒子。藉由該製造方法，可獲得被覆層含有氮化鋁，且平均球形度為預定之高範圍的被覆氧化鋁粒子。藉由本實施形態之氧化鋁粒子包含該被覆氧化鋁粒子，可抑制增黏，並獲得具有高熱傳導性之樹脂組成物及散熱零件。以下進行詳述。(Method of manufacturing coated alumina particles) With regard to the manufacturing method of the coated alumina particles of this embodiment, for example, it can be obtained by using a step including the following steps: In the first step, a mixture containing raw alumina powder and carbon powder is placed in a reducing atmosphere containing nitrogen The first calcined powder is calcined at a temperature above 1500°C and below 1700°C to obtain the first calcined powder; in the second step, the first calcined powder is further calcined in an atmospheric atmosphere at a temperature above 600°C and below 900°C to obtain the present embodiment. Coated alumina particles. With this manufacturing method, it is possible to obtain coated alumina particles whose coating layer contains aluminum nitride and has an average sphericity in a predetermined high range. Since the alumina particles of the present embodiment include the coated alumina particles, it is possible to suppress the increase in viscosity, and to obtain a resin composition and heat dissipation parts with high thermal conductivity. This will be described in detail below.

第1步驟中，首先，使用預定的混合機，將原料氧化鋁粉末與碳粉末以成為預定之混合比的方式進行混合。就混合方法而言，只要將原料氧化鋁粉末與碳粉末均勻地混合，則無特別限定，可使用濕式混合及乾式混合中之任一者。作為如此之混合方法，例如可列舉球磨機混合。原料氧化鋁粉末與碳粉末之混合比，考慮原料氧化鋁粉末與碳粉末之化學計量之混合比，並就反應氣氛之形成的觀點，相對於原料氧化鋁粉末100質量份，碳粉末宜為10質量份以上50質量份以下，為15質量份以上45質量份以下更佳。In the first step, first, using a predetermined mixer, the raw material alumina powder and the carbon powder are mixed in a predetermined mixing ratio. The mixing method is not particularly limited as long as the raw material alumina powder and the carbon powder are uniformly mixed, and any one of wet mixing and dry mixing can be used. As such a mixing method, for example, ball mill mixing can be cited. The mixing ratio of the raw alumina powder and the carbon powder, considering the stoichiometric mixing ratio of the raw alumina powder and the carbon powder, and from the viewpoint of the formation of the reaction atmosphere, relative to 100 parts by mass of the raw alumina powder, the carbon powder It is preferably 10 parts by mass or more and 50 parts by mass or less, more preferably 15 parts by mass or more and 45 parts by mass or less.

就原料氧化鋁粉末而言，例如可使用具有α、γ、θ、及η之結晶結構的各種氧化鋁粒子。該氧化鋁粒子通常為球狀。具體而言，原料氧化鋁粉末中含有的利用上述顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下的氧化鋁粒子之平均球形度通常為0.90以上，宜為0.91以上0.99以下，為0.92以上0.98以下更佳。該平均球形度的上限例如為1.00。藉由平均球形度為上述範圍，具有原料氧化鋁粉末與碳粉末之混合變得更加均勻，反應得到促進的效果。As the raw material alumina powder, for example, various alumina particles having crystal structures of α, γ, θ, and η can be used. The alumina particles are generally spherical. Specifically, the average sphericity of alumina particles having a projected area circle equivalent diameter of 1 μm or more and 300 μm or less contained in the raw alumina powder obtained by the above-mentioned microscope method is usually 0.90 or more, preferably 0.91 or more, 0.99 or less, and 0.92 or more. 0.98 or less is better. The upper limit of the average sphericity is, for example, 1.00. When the average sphericity is in the above range, the mixing of the raw alumina powder and the carbon powder becomes more uniform, and the reaction is promoted.

原料氧化鋁粉末之平均粒徑比起後述碳粉末平均粒徑更大的話，考量上述碳還原氮化反應更容易進行的觀點，宜為25μm以上140μm以下，為30μm以上130μm以下更佳。If the average particle diameter of the raw alumina powder is larger than the average particle diameter of the carbon powder described later, considering that the carbon reduction and nitridation reaction proceeds more easily, it is preferably 25 μm or more and 140 μm or less, and more preferably 30 μm or more and 130 μm or less.

原料氧化鋁粉末的比表面積，宜為0.03m2 /g以上0.30m2 /g以下，為0.05m2 /g以上0.25m2 /g以下更佳。比表面積為上述範圍的話，具有原料氧化鋁粉末與碳粉末之混合變得更加均勻，反應得到促進的效果。The specific surface area of the alumina powder raw material, should of 0.03m 2 / g or more 0.30m 2 / g or less, was 0.05m 2 / g or more 0.25m 2 / g or less more preferably. When the specific surface area is in the above range, the mixing of the raw material alumina powder and the carbon powder becomes more uniform, and the reaction is promoted.

本實施形態之碳粉末，平均粒徑為30nm以上70nm以下，體密度為0.10g/cm3 以上0.20g/cm3 以下，比表面積為20m2 /g以上60m2 /g以下。藉由使用如此之碳粉末，碳粉末大量附著於氧化鋁粒子之表面，又，於在高溫下之原料氧化鋁粉末與氮之反應中，碳粉末作為間隔物發揮作用而可抑制氧化鋁粒子彼此的聚結，可理想地製造球形度高的被覆氧化鋁粒子。The carbon powder of this embodiment has an average particle size of 30 nm or more and 70 nm or less, a bulk density of 0.10 g/cm 3 or more and 0.20 g/cm 3 or less, and a specific surface area of 20 m 2 /g or more and 60 m 2 /g or less. By using such carbon powder, a large amount of carbon powder adheres to the surface of alumina particles. In addition, in the reaction between the raw material alumina powder and nitrogen at high temperature, the carbon powder acts as a spacer to inhibit oxidation The coalescence of aluminum particles can ideally produce coated alumina particles with high sphericity.

碳粉末之平均粒徑，考量改善氧化鋁粒子彼此之聚結防止效果的觀點，宜為35nm以上65nm以下。The average particle diameter of the carbon powder is preferably 35 nm or more and 65 nm or less from the viewpoint of improving the effect of preventing aggregation between alumina particles.

又，碳粉末之體密度為0.10g/cm3 以上0.20g/cm3 以下，宜為0.12g/cm3 以上0.18g/cm3 以下。體密度為上述範圍的話，具有碳粉末更均勻地附著於氧化鋁粒子之表面，反應得到促進的效果。此外，本實施形態中，體密度係利用實施例記載之方法測定。In addition, the bulk density of the carbon powder is 0.10 g/cm 3 or more and 0.20 g/cm 3 or less, preferably 0.12 g/cm 3 or more and 0.18 g/cm 3 or less. When the bulk density is in the above range, the carbon powder adheres to the surface of the alumina particles more uniformly, and the reaction is promoted. In addition, in the present embodiment, the body density is measured by the method described in the examples.

另外，碳粉末的比表面積為20m2 /g以上60m2 /g以下，宜為25m2 /g以上55m2 /g以下。比表面積為上述範圍的話，具有氧化鋁粒子彼此之聚結防止效果得到改善的效果。In addition, the specific surface area of the carbon powder is 20 m 2 /g or more and 60 m 2 /g or less, preferably 25 m 2 /g or more and 55 m 2 /g or less. When the specific surface area is in the above range, there is an effect of improving the effect of preventing agglomeration of alumina particles.

碳粉末之全細孔容積宜為1mL/g以上4mL/g以下，為1.5mL/g以上3mL/g以下更佳。全細孔容積為上述範圍的話，氮氣容易侵入至碳內，碳粉末中更容易進行上述碳還原氮化反應。此外，本實施形態中，全細孔容積係利用實施例記載之方法測定。The total pore volume of the carbon powder is preferably 1 mL/g or more and 4 mL/g or less, more preferably 1.5 mL/g or more and 3 mL/g or less. When the total pore volume is in the above range, nitrogen gas is likely to penetrate into the carbon, and the carbon powder is more likely to undergo the carbon reduction and nitridation reaction. In addition, in this embodiment, the total pore volume is measured by the method described in the examples.

就碳粉末而言，例如可列舉乙炔黑、爐黑、及熱碳黑等碳黑、及粉末石墨。考量純度等的觀點，碳粉末宜為乙炔黑。The carbon powder includes, for example, carbon black such as acetylene black, furnace black, and thermal black, and powder graphite. From the viewpoint of purity, etc., the carbon powder is preferably acetylene black.

第1步驟中，係將上述混合物於含有氮氣之還原氣氛下在1500℃以上1700℃以下之溫度進行煅燒，而獲得第1煅燒粉末。此外，於原料氧化鋁粉末之表面之含有氮化鋁之被覆層的生成，係根據表示碳還原氮化反應之下式進行。 Al2 O3 +3C+N2 →2AlN+3CO 含有氮氣之氣體還原氣氛，例如可藉由使用循環於精製裝置以除去氧及水分的還原氣氛爐而獲得。又，氣體除含有氮氣外，亦可含有二氧化碳氣體等不可避免的成分。In the first step, the above mixture is calcined at a temperature of 1500°C or more and 1700°C or less in a reducing atmosphere containing nitrogen to obtain a first calcined powder. In addition, the formation of the coating layer containing aluminum nitride on the surface of the raw alumina powder is carried out according to the following formula representing the carbon reduction nitridation reaction. Al 2 O 3 +3C+N 2 → 2AlN+3CO A gas reducing atmosphere containing nitrogen can be obtained, for example, by using a reducing atmosphere furnace circulating in a refining device to remove oxygen and moisture. In addition, the gas may contain inevitable components such as carbon dioxide gas in addition to nitrogen.

混合物之煅燒時，將氮氣以1L/分鐘以上10L/分鐘之條件供給至混合物的話，就反應促進性與生產性的觀點，係較佳。更佳為以3L/分鐘以上7L/分鐘之條件供給。When calcining the mixture, if nitrogen is supplied to the mixture at a condition of 1 L/min or more and 10 L/min, it is preferable from the viewpoint of reaction promotion and productivity. It is more preferable to supply at 3L/min or more and 7L/min.

第1步驟中之煅燒溫度，考量控制本實施形態之被覆氧化鋁粒子之被覆層與球形度的觀點，宜為1550℃以上1650℃以下。又，就煅燒時間而言，考慮生產性的話，通常為4小時以上12小時以下。此外，氮氣量越多、煅燒溫度越高、及煅燒時間越長，有被覆層越厚的傾向。The firing temperature in the first step is preferably 1550°C or more and 1650°C or less in consideration of controlling the coating layer and sphericity of the coated alumina particles of this embodiment. In addition, the calcination time is usually 4 hours or more and 12 hours or less in consideration of productivity. In addition, the greater the amount of nitrogen, the higher the firing temperature, and the longer the firing time, the thicker the coating layer tends to be.

第2步驟中，係將第1步驟中獲得之第1煅燒粉末於大氣氣氛下在600℃以上900℃以下之溫度進一步煅燒，而獲得被覆氧化鋁粒子。第2步驟中，藉由將第1煅燒粉末進行煅燒，可除去殘存的碳粉末，而可獲得本實施形態之被覆氧化鋁粒子。 第2步驟中之煅燒溫度，考量控制本實施形態之被覆氧化鋁粒子之碳量的觀點，宜為650℃以上850℃以下。又，就煅燒時間而言，考慮可有效率地除去碳粉末的觀點的話，宜為2小時以上6小時以下。In the second step, the first calcined powder obtained in the first step is further calcined at a temperature of 600°C or more and 900°C or less in an air atmosphere to obtain coated alumina particles. In the second step, by calcining the first calcined powder, the remaining carbon powder can be removed, and the coated alumina particles of this embodiment can be obtained. The calcination temperature in the second step is preferably 650°C or more and 850°C or less in view of controlling the carbon content of the coated alumina particles of this embodiment. In addition, the calcination time is preferably 2 hours or more and 6 hours or less in consideration of the viewpoint that the carbon powder can be efficiently removed.

又，第2步驟中，將第1煅燒粉末進行煅燒時，將空氣以1L/分鐘以上3L/分鐘之條件供給至第1煅燒粉末的話，就控制本實施形態之被覆氧化鋁粒子之碳量的觀點，係較佳。更佳為以1.5L/分鐘以上2.5L/分鐘之條件供給。In the second step, when the first calcined powder is calcined, if air is supplied to the first calcined powder at a condition of 1L/min or more and 3L/min, the carbon content of the coated alumina particles of this embodiment is controlled. The point of view is better. More preferably, it is supplied under the condition of 1.5L/min or more and 2.5L/min.

(氧化鋁粉末之製造方法) 本實施形態之氧化鋁粉末可直接使用1種本實施形態之被覆氧化鋁粒子。又，本實施形態之氧化鋁粉末亦可藉由將2種以上之被覆氧化鋁粒子適當混合而獲得。另外，本實施形態之氧化鋁粉末也可藉由將至少1種之本實施形態之被覆氧化鋁粒子、與其以外之填料等適當混合而獲得。混合方法例如可列舉球磨機混合。(Method of manufacturing alumina powder) As the alumina powder of this embodiment, one type of coated alumina particle of this embodiment can be used as it is. In addition, the alumina powder of this embodiment can also be obtained by appropriately mixing two or more kinds of coated alumina particles. In addition, the alumina powder of this embodiment can also be obtained by appropriately mixing at least one kind of the coated alumina particles of this embodiment, and other fillers and the like. The mixing method includes, for example, ball mill mixing.

[樹脂組成物及其製造方法] 本實施形態之樹脂組成物至少含有樹脂、與本實施形態之氧化鋁粉末。本實施形態之樹脂組成物藉由含有上述氧化鋁粉末，可抑制增黏，且可具有高熱傳導性。[Resin composition and its manufacturing method] The resin composition of this embodiment contains at least resin and the alumina powder of this embodiment. By containing the above-mentioned alumina powder, the resin composition of the present embodiment can suppress thickening and can have high thermal conductivity.

(樹脂) 就樹脂而言，可使用熱塑性樹脂及其寡聚物、彈性體類等各種高分子化合物，例如可使用：環氧樹脂、酚醛樹脂、三聚氰胺樹脂、脲樹脂、不飽和聚酯、胺甲酸酯樹脂、丙烯酸樹脂、及氟樹脂；聚醯亞胺、聚醯胺醯亞胺、及聚醚醯亞胺等聚醯胺；聚對苯二甲酸丁二醇酯、及聚對苯二甲酸乙二醇酯等聚酯；聚苯硫醚、芳香族聚酯、聚碸、液晶聚合物、聚醚碸、聚碳酸酯、馬來醯亞胺改性樹脂、ABS(丙烯腈-丁二烯-苯乙烯)樹脂、AAS(丙烯腈-丙烯酸橡膠-苯乙烯)樹脂、AES(丙烯腈-乙烯-丙烯-二烯橡膠-苯乙烯)樹脂、EVA(乙烯乙酸乙烯酯共聚物)樹脂、及聚矽氧樹脂等。該等樹脂可單獨使用1種，或將2種以上適當混合使用。(Resin) As for resins, various polymer compounds such as thermoplastic resins and oligomers and elastomers can be used. For example, epoxy resins, phenolic resins, melamine resins, urea resins, unsaturated polyesters, urethanes can be used. Resins, acrylic resins, and fluororesins; polyimides, polyimides, and polyetherimides; polybutylene terephthalate, and polyethylene terephthalate Polyesters such as alcohol esters; polyphenylene sulfide, aromatic polyester, polysulfide, liquid crystal polymer, polyether sulfide, polycarbonate, maleimide modified resin, ABS (acrylonitrile-butadiene-benzene Ethylene) resin, AAS (acrylonitrile-acrylic rubber-styrene) resin, AES (acrylonitrile-ethylene-propylene-diene rubber-styrene) resin, EVA (ethylene vinyl acetate copolymer) resin, and silicone Resin etc. These resins can be used individually by 1 type, or 2 or more types can be mixed and used suitably.

該等樹脂之中，考量獲得高散熱特性的觀點，宜為環氧樹脂、酚醛樹脂、胺甲酸酯樹脂、丙烯酸樹脂、氟樹脂、聚醯亞胺、聚苯硫醚、聚碳酸酯、ABS樹脂、及聚矽氧樹脂，為聚矽氧樹脂、環氧樹脂、胺甲酸酯樹脂、及丙烯酸樹脂更佳，為聚矽氧樹脂又更佳。 就聚矽氧樹脂而言，宜使用由具有甲基及苯基等有機基之一液型或二液型加成反應型液狀聚矽氧獲得的橡膠或凝膠。作為如此之橡膠或凝膠，例如可列舉Momentive Performance Materials Japan LLC製的「YE5822A液/YE5822B液(商品名)」、及道康寧東麗公司製的「SE1885A液/SE1885B液(商品名)」等。Among these resins, from the viewpoint of obtaining high heat dissipation characteristics, epoxy resin, phenol resin, urethane resin, acrylic resin, fluororesin, polyimide, polyphenylene sulfide, polycarbonate, and ABS are preferred. The resin and silicone resin are preferably silicone resin, epoxy resin, urethane resin, and acrylic resin, and more preferably silicone resin. As for the silicone resin, it is preferable to use rubber or gel obtained from a one-liquid type or two-liquid type addition reaction type liquid silicone having organic groups such as methyl and phenyl groups. Examples of such rubbers or gels include "YE5822A liquid/YE5822B liquid (trade name)" manufactured by Momentive Performance Materials Japan LLC, and "SE1885A liquid/SE1885B liquid (trade name)" manufactured by Dow Corning Toray.

(氧化鋁粉末及樹脂之含量) 本實施形態之樹脂組成物中，考量改善熱傳導率的觀點，相對於該樹脂組成物之總量，本實施形態之氧化鋁粉末之含量宜為67體積%以上88體積%以下，為71體積%以上85體積%以下更佳。本實施形態之氧化鋁粉末即使填充於樹脂，亦不易增黏，故即使在上述範圍內含有於樹脂組成物中，仍可抑制樹脂組成物之增黏。(Content of alumina powder and resin) In the resin composition of this embodiment, considering the viewpoint of improving thermal conductivity, relative to the total amount of the resin composition, the content of the alumina powder of this embodiment is preferably 67% by volume to 88% by volume, and 71% by volume Above 85% by volume is more preferable. Even if the alumina powder of this embodiment is filled with resin, it is difficult to increase the viscosity, so even if it is contained in the resin composition within the above-mentioned range, the resin composition can still be prevented from increasing the viscosity.

本實施形態之樹脂組成物中，考量樹脂組成物之成形性的觀點，相對於該樹脂組成物之總量，本實施形態之樹脂之含量宜為12體積%以上33體積%以下，為15體積%以上29%以下更佳。In the resin composition of this embodiment, considering the formability of the resin composition, the content of the resin of this embodiment is preferably 12% by volume to 33% by volume, and 15% by volume relative to the total amount of the resin composition. More than 29% is better.

(其他成分) 本實施形態之樹脂組成物中，在不損及本實施形態之特性的範圍內，於本實施形態之氧化鋁粉末及樹脂以外視需要亦可含有：熔融二氧化矽、結晶二氧化矽、鋯石、矽酸鈣、碳酸鈣、碳化矽、氮化鋁、氮化硼、鈹土、及氧化鋯等無機填料；三聚氰胺及苯并胍胺等含氮化合物、含㗁𠯤環之化合物、及磷系化合物之磷酸酯化合物、芳香族縮合磷酸酯、及含鹵素之縮合磷酸酯等阻燃性化合物；添加劑等。作為添加劑，可列舉：馬來酸二甲酯等反應延遲劑、硬化劑、硬化促進劑、阻燃助劑、阻燃劑、著色劑、黏著賦予劑、紫外線吸收劑、抗氧化劑、螢光增白劑、光增感劑、增黏劑、潤滑劑、消泡劑、表面調整劑、光澤劑、及聚合抑制劑等。該等成分可單獨使用1種，或將2種以上適當混合使用。本實施形態之樹脂組成物中，其他成分的含有率通常各自為0.1質量%以上5質量%以下。(Other ingredients) The resin composition of this embodiment may contain fused silica, crystalline silica, and zirconium as needed in addition to the alumina powder and resin of this embodiment, within the range that does not impair the characteristics of this embodiment. Inorganic fillers such as stone, calcium silicate, calcium carbonate, silicon carbide, aluminum nitride, boron nitride, beryllium soil, and zirconium oxide; nitrogen-containing compounds such as melamine and benzoguanamine, compounds containing 㗁𠯤 ring, and phosphorus Flame retardant compounds such as phosphoric acid ester compounds, aromatic condensed phosphoric acid esters, and halogen-containing condensed phosphoric acid esters; additives, etc. Examples of additives include: reaction delay agents such as dimethyl maleate, hardeners, hardening accelerators, flame retardant additives, flame retardants, colorants, adhesion imparting agents, ultraviolet absorbers, antioxidants, and fluorescence enhancement agents. Whitening agents, photosensitizers, tackifiers, lubricants, defoamers, surface modifiers, gloss agents, polymerization inhibitors, etc. These components can be used individually by 1 type, or 2 or more types can be mixed and used suitably. In the resin composition of this embodiment, the content rate of other components is each 0.1 mass% or more and 5 mass% or less normally.

(樹脂組成物之製造方法) 本實施形態之樹脂組成物之製造方法，例如可列舉將樹脂、氧化鋁粉末、及視需要之其他成分進行充分攪拌而獲得的方法。本實施形態之樹脂組成物，例如可藉由將預定量之各成分，利用混摻機及亨舍爾混合機等摻配後，藉由加熱輥、捏合機、及單軸或雙軸擠壓機等混練，冷卻後進行粉碎而製造。(Method of manufacturing resin composition) The method for producing the resin composition of the present embodiment includes, for example, a method obtained by sufficiently stirring resin, alumina powder, and other components as necessary. For the resin composition of this embodiment, for example, a predetermined amount of each component can be blended by a blender, Henschel mixer, etc., and then extruded by a heating roll, a kneader, and uniaxial or biaxial extrusion. It is manufactured by kneading with a machine, cooling, and crushing.

[散熱零件] 本實施形態之散熱零件含有本實施形態之氧化鋁粉末或樹脂組成物。本實施形態之散熱零件藉由使用上述氧化鋁粉末或樹脂組成物，可達成高熱傳導性，亦即可具有高散熱性。就散熱零件而言，例如可列舉散熱片、散熱膏、散熱隔件、半導體密封材、及散熱塗料(散熱塗覆劑)。[Heat Dissipation Parts] The heat dissipating part of this embodiment contains the alumina powder or resin composition of this embodiment. The heat dissipating part of this embodiment can achieve high thermal conductivity by using the above-mentioned alumina powder or resin composition, that is, high heat dissipation. Examples of heat-radiating parts include heat-radiating fins, heat-radiating pastes, heat-radiating spacers, semiconductor sealing materials, and heat-radiating paints (heat-radiating coating agents).

散熱片通常係用以將由發熱性電子零件及電子器件等產生的熱除去之絕緣性的熱傳導性片材。散熱片只要含有本實施形態之氧化鋁粉末或樹脂組成物，則無特別限定。本實施形態之散熱片中含有的氧化鋁粉末以外的材料，例如可列舉聚矽氧橡膠。散熱片主要安裝於散熱鰭片(fin)或金屬板而使用。就散熱片而言，例如可藉由將本實施形態之氧化鋁粉末、與聚矽氧橡膠利用溶劑澆鑄法、及擠壓成膜等方法成形為片狀而獲得。成形為片狀時，宜進行脫泡。散熱片的厚度通常宜為10μm以上300μm以下。The heat sink is generally an insulating thermally conductive sheet used to remove heat generated from heat-generating electronic parts and electronic devices. The heat sink is not particularly limited as long as it contains the alumina powder or resin composition of this embodiment. Examples of materials other than alumina powder contained in the heat sink of this embodiment include silicone rubber. The heat sink is mainly installed on a heat sink fin or a metal plate for use. The heat sink can be obtained, for example, by forming the alumina powder of the present embodiment, and silicone rubber into a sheet by a solvent casting method, extrusion film formation, or the like. When it is formed into a sheet shape, it is advisable to perform defoaming. The thickness of the heat sink is usually 10 μm or more and 300 μm or less.

散熱膏通常塗布於發熱構件與散熱構件之間，且係為了將發熱構件產生的熱有效率地傳導至散熱構件，以促進散熱而使用。散熱膏只要含有本實施形態之氧化鋁粉末或樹脂組成物，則無特別限定。本實施形態之散熱膏中含有的氧化鋁粉末以外的材料，例如可列舉聚矽氧油等有機矽化合物、及聚α-烯烴油等烴系合成油。就散熱膏而言，例如可藉由將本實施形態之氧化鋁粉末分散於有機矽化合物或烴系合成油，製成半固體狀而獲得。又，散熱膏亦可藉由使用將本實施形態之氧化鋁粉末分散於有機矽化合物或烴系合成油而得之樹脂組成物，並將該樹脂組成物製成半固體狀而獲得。The heat-dissipating paste is usually applied between the heat-generating component and the heat-dissipating component, and is used in order to efficiently conduct the heat generated by the heat-generating component to the heat-dissipating component to promote heat dissipation. The heat dissipation paste is not particularly limited as long as it contains the alumina powder or resin composition of this embodiment. Examples of materials other than the alumina powder contained in the heat dissipation paste of the present embodiment include organosilicon compounds such as silicone oil, and hydrocarbon-based synthetic oils such as poly-α-olefin oil. The heat dissipation paste can be obtained, for example, by dispersing the alumina powder of this embodiment in an organosilicon compound or a hydrocarbon-based synthetic oil, and making it into a semi-solid state. In addition, the heat dissipation paste can also be obtained by using a resin composition obtained by dispersing the alumina powder of this embodiment in an organosilicon compound or a hydrocarbon-based synthetic oil, and making the resin composition into a semi-solid state.

散熱隔件通常係為了填埋發熱性電子零件及電子器件、與將該等予以收容之殼體之間的空間而使用。藉由使用該散熱隔件，可將由發熱性電子零件及電子器件等產生的熱直接傳熱至電子設備之殼體等並進行散熱。散熱隔件只要含有本實施形態之氧化鋁粉末或樹脂組成物，則無特別限定。本實施形態之散熱隔件中含有的氧化鋁粉末以外的材料，例如可列舉聚矽氧橡膠。散熱隔件通常可利用與散熱片同樣的方法獲得，但其厚度比起散熱片更厚。The heat-dissipating spacer is generally used to fill the space between the heat-generating electronic parts and electronic devices and the housing in which they are accommodated. By using the heat-dissipating spacer, the heat generated by heat-generating electronic parts and electronic devices can be directly transferred to the housing of electronic equipment, etc. and dissipated. The heat dissipation spacer is not particularly limited as long as it contains the alumina powder or resin composition of this embodiment. Examples of materials other than alumina powder contained in the heat dissipation spacer of this embodiment include silicone rubber. The heat dissipating spacer can usually be obtained by the same method as the heat sink, but its thickness is thicker than that of the heat sink.

半導體密封材係為了將由半導體元件等電子零件產生的熱除去，且保護電子零件免受外部刺激而使用。半導體密封材只要含有本實施形態之氧化鋁粉末或樹脂組成物，則無特別限定。就半導體密封材而言，例如可藉由將本實施形態之氧化鋁粉末或樹脂組成物、與通常使用於密封材料用途之各種公知的添加劑或溶劑等，利用公知的混合器進行混合而製造。混合時之各種成分、溶劑的添加方法可適當使用一般公知的方法，並無特別限定。The semiconductor sealing material is used to remove heat generated from electronic components such as semiconductor elements and to protect the electronic components from external stimuli. The semiconductor sealing material is not particularly limited as long as it contains the alumina powder or the resin composition of this embodiment. The semiconductor sealing material can be produced, for example, by mixing the alumina powder or resin composition of this embodiment with various known additives or solvents generally used for sealing material applications with a known mixer. The method of adding various components and solvents at the time of mixing can appropriately use a generally known method, and is not particularly limited.

散熱塗料係塗布於具有熱源之機械零件、電氣製品、及電氣零件等，並為了提高該等零件等的散熱性而使用。散熱塗料只要含有本實施形態之氧化鋁粉末或樹脂組成物、與溶劑，則無限定。本實施形態之氧化鋁粉末在將氧化鋁粉末填充於樹脂時可抑制黏度上升，故即使在溶劑中仍可維持適合的黏度。就溶劑而言，例如可列舉：水、甲乙酮、甲基異丁基酮、乙酸乙酯、乙酸丙酯、乙酸丁酯、環己酮、乙苯、二甲苯、甲基丙烯酸甲酯、及1-丁醇。該等溶劑可單獨使用1種，或將2種以上適當混合使用。又，機械零件例如可列舉引擎、鍋爐、鼓風機、及泵浦。電氣製品例如可列舉照明、太陽能電池模組、及冰箱。電氣零件例如可列舉電路基板。 [實施例]The heat-dissipating paint is applied to mechanical parts, electrical products, and electrical parts with heat sources, and is used to improve the heat dissipation of these parts. The heat-dissipating paint is not limited as long as it contains the alumina powder or resin composition of this embodiment, and a solvent. The alumina powder of this embodiment can suppress the increase in viscosity when the alumina powder is filled in the resin, and therefore can maintain a suitable viscosity even in a solvent. As for the solvent, for example, water, methyl ethyl ketone, methyl isobutyl ketone, ethyl acetate, propyl acetate, butyl acetate, cyclohexanone, ethylbenzene, xylene, methyl methacrylate, and 1 -Butanol. These solvents may be used individually by 1 type, or may mix and use 2 or more types suitably. In addition, examples of mechanical parts include engines, boilers, blowers, and pumps. Examples of electrical products include lighting, solar cell modules, and refrigerators. Examples of electrical components include circuit boards. [Example]

以下顯示實施例及比較例詳細地說明本發明，但本發明不限定於該等實施例。Examples and comparative examples are shown below to illustrate the present invention in detail, but the present invention is not limited to these examples.

[評價方法] (1)被覆氧化鋁粒子之平均球形度、及比例 使用由氧化鋁粉末利用孔目53μm之JIS規格之不銹鋼製試驗用篩而得之篩上物來分取被覆氧化鋁粒子。 如上述顯微鏡法，將利用掃描式電子顯微鏡(日本電子公司製JSM-6301F型)拍攝之粒子圖像讀入圖像解析裝置(MOUNTECH公司製「MacView Ver. 4」(商品名))，由照片測定粒子之投影面積(A)與周圍長(PM)。使用該等值求出各粒子之球形度及其比例，又，將各粒子之球形度之相加平均值定義為平均球形度。此外，將本實施形態之被覆氧化鋁粒子之SEM圖像(500倍)示於圖1作為參考。[Evaluation method] (1) Average sphericity and ratio of coated alumina particles The coated alumina particles were separated using a sieve obtained from alumina powder using a JIS-standard stainless steel test sieve with a mesh of 53 μm. As in the above-mentioned microscope method, the particle image taken with a scanning electron microscope (JSM-6301F manufactured by JEOL Ltd.) is read into an image analysis device (“MacView Ver. 4” (trade name) manufactured by MOUNTECH), and the photograph is taken Measure the projected area (A) and surrounding length (PM) of the particles. Use these values to find the sphericity of each particle and its ratio, and define the sum of the sphericity of each particle as the average sphericity. In addition, the SEM image (500 times) of the coated alumina particles of this embodiment is shown in FIG. 1 for reference.

(2)平均粒徑及粒度分布(峰部數) 平均粒徑及粒度分布(峰部數)係利用雷射繞射光散射法粒度分布測定裝置(Malvern公司製，產品名「Mastersizer 3000」，濕式分散單元：Hydro MV裝設)進行測定。測定時使用水作為溶劑，就前處理而言使用TOMY精工公司製的超音波發生器UD-200(超微量晶片TP-040裝設)(產品名)施以200W之輸出進行2分鐘分散處理。將分散處理後之粒子以使雷射散射強度成為10～15%的方式滴加至分散單元。分散單元攪拌器之攪拌速度設定為1750rpm，超音波模式設定為無。粒度分布的解析係將粒徑0.01～3500μm之範圍分割成100區段來實施。水的折射率使用1.33，氧化鋁粒子、及被覆氧化鋁粒子的折射率使用1.768。測得之質量基準之粒度分布中，將累積質量成為50%之粒子定義為平均粒徑。又，峰部為於上述粒徑範圍檢測到之極大點。(2) Average particle size and particle size distribution (number of peaks) The average particle size and particle size distribution (number of peaks) were measured by a laser diffraction light scattering method particle size distribution measuring device (manufactured by Malvern, product name "Mastersizer 3000", wet dispersion unit: Hydro MV installation). For the measurement, water was used as a solvent, and the ultrasonic generator UD-200 (ultra-micro wafer TP-040 installation) (product name) manufactured by TOMY Seiko Co., Ltd. was used for the pretreatment, and the output was 200W, and the dispersion treatment was performed for 2 minutes. The particles after the dispersion treatment are dropped into the dispersion unit so that the laser scattering intensity becomes 10-15%. The stirring speed of the dispersing unit stirrer is set to 1750rpm, and the ultrasonic mode is set to none. The analysis of the particle size distribution is performed by dividing the range of the particle size from 0.01 to 3500 μm into 100 segments. 1.33 was used for the refractive index of water, and 1.768 was used for the refractive index of the alumina particles and the coated alumina particles. In the particle size distribution of the measured mass standard, the particles whose cumulative mass becomes 50% are defined as the average particle size. In addition, the peak is the maximum point detected in the above-mentioned particle size range.

(3)被覆氧化鋁粒子中之氮化鋁的含有率 使用由氧化鋁粉末利用孔目53μm之JIS規格之不銹鋼製試驗用篩而得之篩上物來分取被覆氧化鋁粒子。 被覆氧化鋁粒子中之氮化鋁的含有率(以下，亦稱為「AlN含有率」)，係利用粉末X射線繞射圖案之Rietveld解析進行測定。將被覆氧化鋁粒子填入樣品架，使用X射線繞射裝置(Bruker公司製「D8 ADVANCE」(產品名)，檢測器：LynxEye(產品名))測定。測定條件設定為X射線源：CuKα(λ=1.5406Å)、測定法：連續掃描法、掃描速度：0.017°/2.0sec、管電壓：45kV、管電流：360mA、發散狹縫：0.5°、索拉狹縫(soller slit)：4°、測定範圍：2θ=10～70°。根據獲得之X射線繞射圖案，利用使用了解析軟體TOPAS之Rietveld解析所為之定量分析求出氮化鋁的含有率。(3) The content of aluminum nitride in the coated alumina particles The coated alumina particles were separated using a sieve obtained from alumina powder using a JIS-standard stainless steel test sieve with a mesh of 53 μm. The content rate of aluminum nitride in the coated alumina particles (hereinafter also referred to as "AlN content rate") was measured by Rietveld analysis of powder X-ray diffraction patterns. The coated alumina particles are filled in the sample holder, and the measurement is performed using an X-ray diffraction device ("D8 ADVANCE" (product name) manufactured by Bruker, detector: LynxEye (product name)). The measurement conditions were set as X-ray source: CuKα(λ=1.5406Å), measurement method: continuous scanning method, scanning speed: 0.017°/2.0sec, tube voltage: 45kV, tube current: 360mA, divergence slit: 0.5°, cable Soller slit: 4°, measuring range: 2θ=10～70°. Based on the obtained X-ray diffraction pattern, the content rate of aluminum nitride was determined by the quantitative analysis performed by the Rietveld analysis using the analysis software TOPAS.

(4)碳量 使用由氧化鋁粉末利用孔目53μm之JIS規格之不銹鋼製試驗用篩而得之篩上物來分取被覆氧化鋁粒子。 之後，使用碳/硫同時分析計(LECO公司製CS-444LS型(商品名))測定被覆氧化鋁粒子中之碳量，利用檢量線法對碳量進行定量。具體而言，首先，以日本鐵鋼標準試樣之63碳鋼作為標準物質求出檢量線。之後，將實施例及比較例中獲得之被覆氧化鋁粒子0.3g與作為助燃劑之金屬鐵(LECO公司製「IRON CHIP」(產品名))、及金屬鎢(LECO公司製「CECOCEL II」(產品名))一起，於氧氣氣氛下進行氧化燃燒，直到含碳物完全分解，所有碳都轉化為CO2 ，利用紅外檢測器測定生成的CO2 量，求出碳量。(4) Carbon content A sieve obtained from alumina powder using a JIS-standard stainless steel test sieve with a mesh size of 53 μm was used to separate the coated alumina particles. After that, the amount of carbon in the coated alumina particles was measured using a simultaneous carbon/sulfur analyzer (CS-444LS model (trade name) manufactured by LECO), and the amount of carbon was quantified by the calibration curve method. Specifically, first, a calibration curve is obtained using 63 carbon steel, which is a standard sample of Japanese iron and steel, as a standard material. After that, 0.3 g of the coated alumina particles obtained in the Examples and Comparative Examples were combined with metallic iron (“IRON CHIP” (product name) manufactured by LECO Corporation) and tungsten (“CECOCEL II” manufactured by LECO Corporation) as a combustion enhancer. product name)) together with an oxidation combustion in oxygen atmosphere until complete decomposition of the carbonaceous material, all carbons are converted, the amount of CO 2 measured using an infrared detector to generate CO 2, the amount of carbon determined.

(5)被覆層的厚度 使用由氧化鋁粉末利用孔目53μm之JIS規格之不銹鋼製試驗用篩而得之篩上物來分取被覆氧化鋁粒子。 如圖1所示，被覆氧化鋁粒子中之被覆層的厚度係利用剖面EPMA分析進行測定。首先，將被覆氧化鋁粒子包埋於G-2環氧樹脂(Gatan公司製)，剖面研磨後實施鋨塗覆。將塗覆後之樣品利用電子微探儀(日本電子公司製JXA-8230(產品名))進行N元素的分佈分析(mapping analysis)。加速電壓設定為15kV，照射電流設定為5×10-8 A。將獲得之分佈圖像讀入圖像解析裝置(MOUNTECH公司製「MacView Ver. 4」(商品名))，求出被覆層的厚度。針對1個粒子，求出10處的厚度，將其相加平均值定義為1個粒子之被覆層的厚度。求得以此種方式獲得之200個任意粒子之被覆層的厚度，將其相加平均值定義為被覆氧化鋁粒子中之被覆層的厚度。(5) The thickness of the coating layer A sieve obtained from alumina powder using a JIS-standard stainless steel test sieve with a mesh of 53 μm was used to separate the coated alumina particles. As shown in Fig. 1, the thickness of the coating layer in the coated alumina particles was measured by cross-sectional EPMA analysis. First, the coated alumina particles are embedded in G-2 epoxy resin (manufactured by Gatan Corporation), and the cross-section is polished, followed by osmium coating. The coated sample was subjected to a mapping analysis of the N element using an electronic microprobe (JXA-8230 (product name) manufactured by JEOL Ltd.). The acceleration voltage is set to 15kV, and the irradiation current is set to 5×10 -8 A. The obtained distribution image was read into an image analysis device (“MacView Ver. 4” (trade name) manufactured by MOUNTECH Corporation), and the thickness of the coating layer was determined. For one particle, the thickness of 10 locations is obtained, and the average value of the addition is defined as the thickness of the coating layer of one particle. Calculate the thickness of the coating layer of 200 arbitrary particles obtained in this way, and define the average value thereof as the thickness of the coating layer in the coated alumina particles.

(6)比表面積 使用由氧化鋁粉末利用孔目53μm之JIS規格之不銹鋼製試驗用篩而得之篩上物來分取被覆氧化鋁粒子。 比表面積的測定係使用Macsorb公司製HM-model 1208進行。在測定前，於氮氣氣氛中以300℃、18分鐘之條件進行加熱，實施被覆氧化鋁粒子之前處理。此外，吸附氣體使用氮氣30%、氦氣70%之混合氣體，以使本體流量計之指示值成為25ml/min的方式調整流量。(6) Specific surface area The coated alumina particles were separated using a sieve obtained from alumina powder using a JIS-standard stainless steel test sieve with a mesh of 53 μm. The measurement of the specific surface area was performed using HM-model 1208 manufactured by Macsorb Corporation. Before the measurement, heating was carried out at 300°C for 18 minutes in a nitrogen atmosphere, and the pretreatment for coating the alumina particles was performed. In addition, the adsorption gas uses a mixed gas of 30% nitrogen and 70% helium, and the flow rate is adjusted so that the indication value of the main body flowmeter becomes 25ml/min.

(7)體密度 碳粉末之體密度係依據JIS K 5101-12-2進行測定。(7) Bulk density The bulk density of carbon powder is measured in accordance with JIS K 5101-12-2.

(8)全細孔容積 碳粉末之全細孔容積係利用使用了細孔分布測定裝置(島津製作所公司製AutoPore IV 9520型(商品名))之汞壓入法進行測定。(8) Total pore volume The total pore volume of the carbon powder was measured by a mercury intrusion method using a pore distribution measuring device (AutoPore IV 9520 (trade name) manufactured by Shimadzu Corporation).

(9)氧化鋁粉末中之氧化鋁與氮化鋁之合計含有率 氧化鋁粉末中之氧化鋁與氮化鋁之合計含有率(以下，亦稱為「合計含有率」。)，係利用粉末X射線繞射圖案之Rietveld解析進行測定。以與上述氧化鋁粉末中之氮化鋁的含有率同樣的步驟實施X射線繞射測定，根據獲得之X射線繞射圖案，利用使用了解析軟體TOPAS之Rietveld解析所為之定量分析求出氧化鋁與氮化鋁的含有率。(9) The total content of alumina and aluminum nitride in alumina powder The total content rate of alumina and aluminum nitride in the alumina powder (hereinafter also referred to as "total content rate") is measured by Rietveld analysis of powder X-ray diffraction patterns. The X-ray diffraction measurement was carried out in the same procedure as the content of aluminum nitride in the alumina powder. Based on the obtained X-ray diffraction pattern, the aluminum oxide was obtained by quantitative analysis by Rietveld analysis using analysis software TOPAS And the content of aluminum nitride.

(10)黏度 將實施例及比較例中獲得之氧化鋁粉末投入聚矽氧油(信越化學工業公司製「KF96-100cs」(產品名))中，以使氧化鋁粉末之填充率成為75vol%。將其使用自轉-公轉轉混合器(THINKY公司製「Awatori Kentaro ARE-310」(產品名))以轉速2200rpm混合30秒後，進行真空脫泡，得到樹脂組成物。對獲得之樹脂組成物使用流變儀(Anton-Paar公司製「MCR102」(產品名))測定剪切黏度。測定條件設定為溫度：30℃、板：φ25mm平行板、間隙：1mm。邊使剪切速度從0.01s-1 連續地變化為10s-1 邊進行測定，讀取5s-1 時之黏度。(10) Viscosity Put the alumina powder obtained in the examples and comparative examples into polysiloxane oil ("KF96-100cs" (product name) manufactured by Shin-Etsu Chemical Co., Ltd.) so that the filling rate of the alumina powder becomes 75vol% . This was mixed with a rotation-revolution mixer ("Awatori Kentaro ARE-310" (product name) manufactured by THINKY) at a rotation speed of 2200 rpm for 30 seconds, and then vacuum degassed to obtain a resin composition. A rheometer ("MCR102" (product name) manufactured by Anton-Paar Corporation) was used to measure the shear viscosity of the obtained resin composition. The measurement conditions were set to temperature: 30°C, plate: φ25 mm parallel plate, and gap: 1 mm. Measure while continuously changing the shear rate from 0.01 s -1 to 10 s -1 and read the viscosity at 5 s -1.

(11)熱傳導率 將實施例及比較例中獲得之氧化鋁粉末投入聚矽氧樹脂(道康寧東麗公司製SE-1885A液、及B液)中，以使氧化鋁粉末之填充率成為80vol%。將其攪拌混合後，進行真空脫泡並加工成厚度3mm後，於120℃加熱5小時，得到樹脂組成物。將獲得之樹脂組成物使用熱傳導率測定裝置(Hitachi Technologies and Services公司製樹脂材料熱阻測定裝置「TRM-046RHHT」(產品名))，以依據ASTM D5470之穩態法測定熱傳導率。樹脂組成物加成寬10mm×10mm，邊施以2N之荷重邊實施測定。(11) Thermal conductivity The alumina powders obtained in the examples and comparative examples were put into polysiloxane resin (SE-1885A and B, manufactured by Dow Corning Toray Co., Ltd.) so that the filling rate of the alumina powder became 80 vol%. After stirring and mixing the mixture, vacuum degassing and processing to a thickness of 3 mm, it was heated at 120°C for 5 hours to obtain a resin composition. The obtained resin composition was measured for thermal conductivity by a steady-state method based on ASTM D5470 using a thermal conductivity measuring device (Hitachi Technologies and Services, a resin material thermal resistance measuring device "TRM-046RHHT" (product name)). The resin composition had an added width of 10 mm×10 mm, and the measurement was performed while applying a load of 2N.

[實施例1] 實施例1中，使用Denka(股)公司製DAW-90(產品名)(平均球形度：0.91、平均粒徑：91μm、比表面積：0.1m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末。 又，使用Denka(股)公司製HS-100(產品名)(平均粒徑：46nm、體密度：0.15g/cm3 、比表面積：40m2 /g、全細孔容積：2.1mL/g)作為係碳粉末之乙炔黑。 將原料之氧化鋁粉末50g、與碳粉末20g利用球磨機混合，以7L/min之量供給氮氣，在氮氣氣氛中以煅燒溫度1650℃、及煅燒時間12小時之條件進行煅燒(第1步驟)。之後，以2L/min之量供給空氣，在大氣氣氛中以煅燒溫度700℃、及煅燒時間4小時之條件進行煅燒，得到被覆氧化鋁粒子A。針對被覆氧化鋁粒子A，測定1μm以上300μm以下之被覆氧化鋁粒子之平均球形度、球形度為0.80以下之被覆氧化鋁粒子的比例、平均球形度、相對於全體之AlN的含有率、被覆層的厚度，結果示於表1。 依表1所示之比例(體積%)，摻合作為超微粉之氧化鋁1之住友化學(股)公司製AA-05(產品名)、作為微粉之氧化鋁2之Denka(股)公司製DAW-07(產品名)、作為粗粉之氧化鋁3之被覆氧化鋁粒子A，製成氧化鋁粉末。評價獲得之氧化鋁粉末的物性，結果示於表1。[Example 1] In Example 1, DAW-90 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.91, average particle size: 91 μm, specific surface area: 0.1 m 2 /g) was used as the coated alumina Alumina powder used as a raw material for the manufacture of particles. In addition, HS-100 (product name) manufactured by Denka Co., Ltd. was used (average particle size: 46 nm, bulk density: 0.15 g/cm 3 , specific surface area: 40 m 2 /g, total pore volume: 2.1 mL/g) Acetylene black as a carbon powder. Mix 50g of the raw material alumina powder and 20g of carbon powder with a ball mill, supply nitrogen at a rate of 7L/min, and calcinate in a nitrogen atmosphere at a calcination temperature of 1650°C and a calcination time of 12 hours (Step 1) . After that, air was supplied in an amount of 2 L/min, and calcined under the conditions of a calcining temperature of 700° C. and a calcining time of 4 hours in an air atmosphere to obtain coated alumina particles A. For the coated alumina particles A, measure the average sphericity of the coated alumina particles of 1 μm or more and 300 μm or less, the ratio of the coated alumina particles with the sphericity of 0.80 or less, the average sphericity, the content of AlN relative to the whole, and the coating layer The results are shown in Table 1. According to the ratio shown in Table 1 (vol%), it is made by Sumitomo Chemical Co., Ltd. AA-05 (product name) mixed with alumina 1 as ultrafine powder, and manufactured by Denka Co., Ltd. 2 as fine powder alumina DAW-07 (product name), the coated alumina particles A of alumina 3 as coarse powder, were made into alumina powder. The physical properties of the obtained alumina powder were evaluated, and the results are shown in Table 1.

[實施例2] 實施例2中，使用Denka(股)公司製DAW-70(產品名)(平均球形度：0.92、平均粒徑：70μm、比表面積：0.1m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，並將第1步驟之煅燒溫度變更為1550℃，煅燒時間變更為4小時，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子B。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-05(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子B作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 2] In Example 2, DAW-70 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.92, average particle size: 70 μm, specific surface area: 0.1 m 2 /g) was used as the coated alumina The aluminum oxide powder used as the raw material for the production of the particles, and the calcination temperature in the first step was changed to 1550°C, and the calcination time was changed to 4 hours, except that the same method as in Example 1 was used to produce coated alumina particles B . The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-05 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particles B were used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例3] 實施例3中，使用Denka(股)公司製DAS-30(產品名)(平均球形度：0.93、平均粒徑：30μm、比表面積：0.2m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，將第1步驟之煅燒溫度變更為1500℃，煅燒時間變更為4小時，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子C。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-05(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子C作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 3] In Example 3, DAS-30 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.93, average particle size: 30 μm, specific surface area: 0.2 m 2 /g) was used as the coated alumina For the alumina powder used as the raw material for the production of the particles, the calcination temperature in the first step was changed to 1500°C and the calcination time was changed to 4 hours. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-05 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particles C were used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例4] 實施例4中，使用Denka(股)公司製DAW-120(產品名)(平均球形度：0.91、平均粒徑：115μm、比表面積：0.1m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子D。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-10(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子D作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 4] In Example 4, DAW-120 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.91, average particle size: 115 μm, specific surface area: 0.1 m 2 /g) was used as the coated alumina Except for the alumina powder used as the raw material for the production of the particles, the coated alumina particles D were produced by the same method as in Example 1. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-10 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particle D was used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例5] 實施例5中，將第1步驟之煅燒溫度變更為1600℃，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子E。實施與實施例1同樣的測定，結果示於表1。 使用被覆氧化鋁粒子E作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 5] In Example 5, the calcination temperature in the first step was changed to 1600°C, and the coated alumina particles E were produced by the same method as in Example 1, except that the firing temperature was changed to 1600°C. The same measurement as in Example 1 was performed, and the results are shown in Table 1. Except for using the coated alumina particles E as the coarse powder of alumina 3, the same procedure as in Example 1 was carried out, and the blending (vol%) shown in Table 1 was performed to obtain alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例6] 實施例6中，使用Denka(股)公司製DAW-45(產品名)(平均球形度：0.92、平均粒徑：43μm、比表面積：0.2m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，將第1步驟之煅燒溫度變更為1600℃，煅燒時間變更為8小時，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子F。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-05(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子F作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 6] In Example 6, DAW-45 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.92, average particle size: 43 μm, specific surface area: 0.2 m 2 /g) was used as the coated alumina As for the alumina powder used as the raw material for the production of particles, the calcination temperature in the first step was changed to 1600° C., and the calcination time was changed to 8 hours. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-05 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particle F was used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例7] 實施例7中，使用Denka(股)公司製DAW-70(產品名)(平均球形度：0.92、平均粒徑：70μm、比表面積：0.1m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，將第1步驟之煅燒溫度變更為1600℃，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子G。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-05(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子G作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 7] In Example 7, DAW-70 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.92, average particle size: 70 μm, specific surface area: 0.1 m 2 /g) was used as the coated alumina As for the alumina powder used as the raw material for the production of the particles, the calcination temperature in the first step was changed to 1600°C, and the coated alumina particles G were produced by the same method as in Example 1. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-05 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particles G were used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例8] 實施例8中，使用Denka(股)公司製DAW-120(產品名)(平均球形度：0.91、平均粒徑：115μm、比表面積：0.1m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，將第1步驟之煅燒溫度變更為1600℃，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子H。實施與實施例1同樣的測定，結果示於表1。 使用Denka(股)公司製DAW-10(產品名)作為微粉之氧化鋁2，並使用被覆氧化鋁粒子H作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Example 8] In Example 8, DAW-120 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.91, average particle size: 115 μm, specific surface area: 0.1 m 2 /g) was used as the coated alumina The alumina powder used as the raw material for the production of the particles was changed to 1600° C. in the first step, and the coated alumina particles H were produced by the same method as in Example 1 except that the firing temperature was changed to 1600°C. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The same procedure as in Example 1 was carried out except that DAW-10 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particles H were used as the coarse powder of alumina 3, according to Table 1. The indicated blending (vol%) gives alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[實施例9] 將氧化鋁之摻合比變更為表1所示之比例(體積%)，除此以外，與實施例7同樣進行，製造氧化鋁粉末並進行評價。結果示於表1。[Example 9] Except that the blending ratio of alumina was changed to the ratio (vol%) shown in Table 1, the same procedure as in Example 7 was carried out, and alumina powder was produced and evaluated. The results are shown in Table 1.

[實施例10] 將氧化鋁之摻合比變更為表1所示之比例(體積%)，除此以外，與實施例7同樣進行，製造氧化鋁粉末並進行評價。結果示於表1。[Example 10] Except that the blending ratio of alumina was changed to the ratio (vol%) shown in Table 1, the same procedure as in Example 7 was carried out, and alumina powder was produced and evaluated. The results are shown in Table 1.

[比較例1] 比較例1中，使用Denka(股)公司製DAW-05(產品名)作為微粉之氧化鋁2，並使用Denka(股)公司製DAW-45(產品名)(平均球形度：0.92、平均粒徑：43μm、比表面積：0.2m2 /g)替代被覆氧化鋁粒子A作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Comparative Example 1] In Comparative Example 1, DAW-05 (product name) manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2, and DAW-45 (product name) manufactured by Denka Co., Ltd. (product name) was used (average sphericity) : 0.92, average particle size: 43μm, specific surface area: 0.2m 2 /g), except that the coated alumina particle A is used as the coarse powder of alumina 3, the same procedure as in Example 1 is carried out, and the blending is shown in Table 1. Combined (vol%) to obtain alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[比較例2] 比較例2中，使用Denka(股)公司製DAW-45(產品名)(平均球形度：0.92、平均粒徑：43μm、比表面積：0.2m2 /g)作為被覆氧化鋁粒子之製造所使用之原料之氧化鋁粉末，將第1步驟之煅燒溫度變更為1650℃，煅燒時間變更為30小時，除此以外，利用與實施例1同樣之方法製造被覆氧化鋁粒子a。實施與實施例1同樣的測定，結果示於表1。被覆氧化鋁粒子a不屬於本實施形態之被覆氧化鋁粒子。 使用Denka(股)公司製DAW-05作為微粉之氧化鋁2，並使用被覆氧化鋁粒子a作為粗粉之氧化鋁3，除此以外，與實施例1同樣進行，依表1所示之摻合(體積%)得到氧化鋁粉末。又，實施與實施例1同樣的測定，結果示於表1。[Comparative Example 2] In Comparative Example 2, DAW-45 (product name) manufactured by Denka Co., Ltd. (average sphericity: 0.92, average particle size: 43 μm, specific surface area: 0.2 m 2 /g) was used as the coated alumina As for the alumina powder used as the raw material for the production of the particles, the calcination temperature in the first step was changed to 1650°C and the calcination time was changed to 30 hours. The same measurement as in Example 1 was performed, and the results are shown in Table 1. The coated alumina particles a do not belong to the coated alumina particles of this embodiment. The same procedure as in Example 1 was performed except that DAW-05 manufactured by Denka Co., Ltd. was used as the fine powder of alumina 2 and the coated alumina particle a was used as the coarse powder of alumina 3, and the blending was as shown in Table 1. Combined (vol%) to obtain alumina powder. In addition, the same measurement as in Example 1 was performed, and the results are shown in Table 1.

[表1]

Figure 02_image001
[Table 1]
Figure 02_image001

本申請係基於2019年5月30日提申之日本專利申請案(特願2019-101604)，其內容援引於此作為參照。This application is based on a Japanese patent application (Japanese Patent Application No. 2019-101604) filed on May 30, 2019, and the content is incorporated herein by reference.

[產業上利用性] 根據本發明之被覆氧化鋁粉末，填充於樹脂時可抑制黏度上升，且可達成含有該樹脂之樹脂組成物的高熱傳導化。因此，例如於散熱片、散熱膏、散熱隔件、半導體密封材、及散熱塗料(散熱塗覆劑)等散熱零件之用途特別有用。[Industrial Utilization] According to the coated alumina powder of the present invention, the increase in viscosity can be suppressed when the resin is filled, and high thermal conductivity of the resin composition containing the resin can be achieved. Therefore, it is particularly useful for heat dissipation components such as heat sinks, heat dissipation pastes, heat dissipation spacers, semiconductor sealing materials, and heat dissipation paints (heat dissipation coating agents).

[圖1]本實施形態之被覆氧化鋁粒子之剖面EPMA分析的圖像。[Figure 1] EPMA analysis image of the cross-section of the coated alumina particles of this embodiment.

Claims (10)

一種氧化鋁粉末，含有被覆氧化鋁粒子，該被覆氧化鋁粒子具有氧化鋁粒子、及將該氧化鋁粒子予以被覆之被覆層，且利用顯微鏡法獲得之投影面積圓相當徑為1μm以上300μm以下；該被覆層含有氮化鋁；及該被覆氧化鋁粒子之平均球形度為0.85以上0.97以下；該被覆氧化鋁粒子中之氮化鋁的含有率為15質量%以上40質量%以下。 An alumina powder containing coated alumina particles, the coated alumina particles having alumina particles and a coating layer covering the alumina particles, and the equivalent diameter of the projected area circle obtained by a microscope is 1 μm or more and 300 μm or less; The coating layer contains aluminum nitride; and the average sphericity of the coated alumina particles is 0.85 or more and 0.97 or less; the content of aluminum nitride in the coated alumina particles is 15% by mass or more and 40% by mass or less. 如請求項1之氧化鋁粉末，其中，該氧化鋁粉末之利用雷射繞射散射法獲得之體積基準頻率粒度分布中，於粒徑為2μm以上200μm以下之粒度範圍具有多個峰部。 The alumina powder of claim 1, wherein the volume-based frequency particle size distribution of the alumina powder obtained by the laser diffraction scattering method has multiple peaks in the particle size range of 2 μm or more and 200 μm or less. 如請求項1或2之氧化鋁粉末，其中，該被覆氧化鋁粒子中，球形度為0.80以下之被覆氧化鋁粒子的比例以個數基準計為15%以下。 The alumina powder of claim 1 or 2, wherein the proportion of coated alumina particles having a sphericity of 0.80 or less in the coated alumina particles is 15% or less based on the number. 如請求項1或2之氧化鋁粉末，其中，利用雷射繞射散射式粒度分布測定儀測得的該被覆氧化鋁粒子之平均粒徑為30μm以上150μm以下。 The alumina powder of claim 1 or 2, wherein the average particle diameter of the coated alumina particles measured by a laser diffraction scattering particle size distribution analyzer is 30 μm or more and 150 μm or less. 如請求項1或2之氧化鋁粉末，其中，該氧化鋁粉末中之氧化鋁與氮化鋁之合計含有率為80質量%以上。 The alumina powder of claim 1 or 2, wherein the total content of alumina and aluminum nitride in the alumina powder is 80% by mass or more. 如請求項1或2之氧化鋁粉末，其中，該被覆氧化鋁粒子中之碳量為0.3質量%以下。 The alumina powder of claim 1 or 2, wherein the amount of carbon in the coated alumina particles is 0.3% by mass or less. 一種樹脂組成物，含有樹脂、及如請求項1至6中之任一項之氧化鋁粉末。 A resin composition containing resin and alumina powder according to any one of claims 1 to 6. 如請求項7之樹脂組成物，其中，該樹脂含有選自由聚矽氧樹脂、環氧樹脂、胺甲酸酯樹脂、及丙烯酸樹脂構成之群組中之至少1種。 The resin composition of claim 7, wherein the resin contains at least one selected from the group consisting of silicone resin, epoxy resin, urethane resin, and acrylic resin. 一種散熱零件，含有如請求項1至6中之任一項之氧化鋁粉末、或如請求項7或8之樹脂組成物。 A heat-dissipating component containing the alumina powder according to any one of claims 1 to 6, or the resin composition according to claim 7 or 8. 一種如請求項1之被覆氧化鋁粒子之製造方法，包含下列步驟：第1步驟，將含有原料之氧化鋁粉末與碳粉末的混合物於含有氮氣之還原氣氛下在1500℃以上1700℃以下之溫度進行煅燒，而獲得第1煅燒粉末；及第2步驟，將該第1煅燒粉末於大氣氣氛下在600℃以上900℃以下之溫度進一步煅燒，而獲得該被覆氧化鋁粒子；該碳粉末之平均粒徑為30nm以上70nm以下，體密度(bulk density)為0.10g/cm3以上0.20g/cm3以下，及比表面積為20m2/g以上60m2/g以下。 A method for manufacturing coated alumina particles according to claim 1, comprising the following steps: the first step is to place a mixture of alumina powder and carbon powder containing raw materials in a reducing atmosphere containing nitrogen at a temperature of 1500°C or more and 1700°C or less Calcining at a temperature to obtain the first calcined powder; and in the second step, the first calcined powder is further calcined at a temperature of 600°C or more and 900°C or less in an air atmosphere to obtain the coated alumina particles; the carbon powder The average particle size is 30nm or more and 70nm or less, the bulk density is 0.10g/cm 3 or more and 0.20g/cm 3 or less, and the specific surface area is 20m 2 /g or more and 60m 2 /g or less.
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TW201132579A (en) * 2010-01-29 2011-10-01 Tokuyama Corp Process for production of spherical aluminum nitride powder, and spherical aluminum nitride powder produced by the process

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