TWI674251B - Aluminum-carbonized tantalum composite and manufacturing method thereof - Google Patents
Aluminum-carbonized tantalum composite and manufacturing method thereof Download PDFInfo
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Abstract
提供一種高導熱、低熱膨脹且低比重的鋁-碳化矽質複合體及其製造方法。 Provided is an aluminum-silicon carbide composite with high thermal conductivity, low thermal expansion, and low specific gravity, and a method for manufacturing the same.
提供一種鋁-碳化矽質複合體，係將鋁合金含浸於多孔質碳化矽成形體而成，該鋁-碳化矽質複合體之特徵為：該複合體中碳化矽的比例為60體積%以上，含有60質量%以上75質量%以下之粒徑為80μm以上800μm以下的碳化矽，含有20質量%以上30質量%以下之粒徑為8μm以上且小於80μm的碳化矽，含有5質量%以上10質量%以下之粒徑為小於8μm的碳化矽。 Provided is an aluminum-silicon carbide composite, which is made by impregnating an aluminum alloy with a porous silicon carbide compact. The aluminum-silicon carbide composite is characterized in that the proportion of silicon carbide in the composite is 60% by volume or more. , Containing 60% by mass to 75% by mass of silicon carbide having a particle size of 80 μm to 800 μm, containing 20% by mass to 30% by mass of silicon carbide having a particle size of 8 μm or more and less than 80 μm, containing 5% by mass or more 10 The silicon carbide having a particle diameter of less than 8% by mass is less than 8 μm.
Description
本發明係有關鋁-碳化矽質複合體及其製造方法。 The invention relates to an aluminum-silicon carbide composite and a manufacturing method thereof.
自昔以來，在電源模組中的散熱材方面，係一直使用銅到現在。然而，在將銅作為散熱材使用的情況，由於其高熱膨脹係數(17ppm/K)的緣故，搭載於散熱材上的陶瓷電路基板將兩者接合的銲料上會產生裂痕等，而在可靠性方面成為問題。因此，被期望具低熱膨脹、高導熱性的散熱材。 In the past, copper has been used as a heat sink in power modules until now. However, when copper is used as a heat sink, due to its high coefficient of thermal expansion (17ppm / K), cracks and the like may occur on the solder of the ceramic circuit board mounted on the heat sink to join the two, which results in reliability. Aspect becomes a problem. Therefore, a heat sink having low thermal expansion and high thermal conductivity is desired.
在上述狀況下，由於碳化矽質複合體係可藉由提高該複合體中碳化矽的含量而將熱膨脹係數抑制在10ppm/K以下，且可顯現高導熱性及低比重等考量，故近年來被作為散熱材而受到矚目(專利文獻1、2及3)。 Under the above conditions, the silicon carbide composite system can suppress the thermal expansion coefficient below 10 ppm / K by increasing the content of silicon carbide in the composite, and can take into consideration considerations such as high thermal conductivity and low specific gravity. It has attracted attention as a heat sink (Patent Documents 1, 2 and 3).
但是，習知的碳化矽質複合體的導熱係數在室溫下充其量均為200W/mK左右，不及於銅的(400W/mK)，而企盼具有更高導熱係數的碳化矽質複合體。 However, the thermal conductivity of conventional silicon carbide composites is at best about 200 W / mK at room temperature, which is inferior to that of copper (400 W / mK), and silicon carbide composites with higher thermal conductivity are expected.
本發明者們為解決習知的散熱材所具有的課題，經反覆專心致力檢討的結果發現到：碳化矽質複合體的導熱係數是大大地取決於構成該複合體之碳化矽粒 子的粒徑和碳化矽的含量，又，具有特定範圍的粒徑及碳化矽含量的複合體會呈現230W/mK以上的高導熱係數，而且，僅使用粒徑大的碳化矽粉末並不會增加複合體中的碳化矽含量因而無法達成230W/mK以上的高導熱係數，此外，在以使碳化矽含量增加之目的而添加碳化矽的微粉時，為達成230W/mK以上的高導熱係數，應特定所使用的碳化矽粒子的粒徑及其量，遂完成本發明。 In order to solve the problems of the conventional heat-dissipating materials, the present inventors have repeatedly focused on the review and found that the thermal conductivity of the silicon carbide composite depends greatly on the silicon carbide particles constituting the composite. Particle size and silicon carbide content, and a composite with a specific range of particle size and silicon carbide content will exhibit a high thermal conductivity of more than 230W / mK, and only using silicon carbide powder with a large particle size will not increase Therefore, the silicon carbide content in the composite cannot achieve a high thermal conductivity of more than 230 W / mK. In addition, when adding silicon carbide fine powder for the purpose of increasing the silicon carbide content, in order to achieve a high thermal conductivity of 230 W / mK or more, The particle diameter and the amount of the silicon carbide particles used were specified, and the present invention was completed.
[專利文獻1]日本特開2000-154080號公報 [Patent Document 1] Japanese Patent Laid-Open No. 2000-154080
[專利文獻2]日本特開2000-141022號公報 [Patent Document 2] Japanese Patent Laid-Open No. 2000-141022
[專利文獻3]日本特開2000-169267號公報 [Patent Document 3] Japanese Patent Laid-Open No. 2000-169267
本發明係有鑑於上述事情而完成者，目的在於可獲得高導熱、低熱膨脹且低比重的鋁-碳化矽質複合體。 The present invention has been made in view of the foregoing, and an object thereof is to obtain an aluminum-silicon carbide composite having high thermal conductivity, low thermal expansion, and low specific gravity.
本發明的鋁-碳化矽質複合體，係將鋁合金含浸於多孔質碳化矽成形體而成，該鋁-碳化矽質複合體之特徵為：該複合體中碳化矽的比例為60體積%以上，含有60質量%以上75質量%以下之粒徑為80μm以上800μm以下的碳化矽，含有20質量%以上30質量%以下之粒徑為8μm以上且小於80μm的碳化矽，含有5質量%以上10質量%以下之粒徑為小於8μm的碳化矽。 The aluminum-silicon carbide composite of the present invention is made by impregnating an aluminum alloy with a porous silicon carbide compact. The aluminum-silicon carbide composite is characterized in that the proportion of silicon carbide in the composite is 60% by volume. Above, containing 60% by mass to 75% by mass of silicon carbide having a particle size of 80 μm to 800 μm, containing 20% by mass to 30% by mass of silicon carbide having a particle size of 8 μm or more and less than 80 μm, containing 5% by mass or more 10% by mass or less of silicon carbide having a particle diameter of less than 8 μm.
依據本發明的一態樣，上述鋁-碳化矽質複合 體之特徵為：在25℃下的導熱係數為230W/mK以上。 According to one aspect of the present invention, the aluminum-silicon carbide composite described above The body is characterized by a thermal conductivity of 230 W / mK or more at 25 ° C.
依據本發明的一態樣，上述鋁-碳化矽質複合體之特徵為：在25℃至150℃中之熱膨脹係數為7.0ppm/K以下。 According to one aspect of the present invention, the aluminum-silicon carbide composite is characterized in that the thermal expansion coefficient at 25 ° C to 150 ° C is 7.0 ppm / K or less.
依據本發明的一態樣，上述鋁-碳化矽質複合體之特徵為：前述鋁合金係含有10質量%~14質量%的矽與0.5質量%~2.5質量%的鎂而成。 According to one aspect of the present invention, the aluminum-silicon carbide composite is characterized in that the aluminum alloy is made of 10% to 14% by mass of silicon and 0.5% to 2.5% by mass of magnesium.
依據本發明的一態樣，上述鋁-碳化矽質複合體之特徵為：係於摻合具有不同粒度分布的3種以上的碳化矽粉末之原料粉末中添加無機接合劑，且經過成形步驟及燒結步驟。 According to one aspect of the present invention, the aluminum-silicon carbide composite is characterized in that an inorganic bonding agent is added to a raw material powder blended with three or more silicon carbide powders having different particle size distributions, and after the forming step and Sintering step.
依據本發明的鋁-碳化矽質複合體或本發明的製造方法所提供之鋁-碳化矽質複合體係高導熱、低熱膨脹且低比重。 The aluminum-silicon carbide composite according to the present invention or the aluminum-silicon carbide composite system provided by the manufacturing method of the present invention has high thermal conductivity, low thermal expansion, and low specific gravity.
以下，就本發明的鋁-碳化矽質複合體及其製造方法，說明一實施形態。惟本發明當然不受限於以下的實施形態。 Hereinafter, an embodiment of the aluminum-silicon carbide composite and its manufacturing method according to the present invention will be described. However, the present invention is not limited to the following embodiments.
本實施形態的鋁-碳化矽質複合體，係將鋁合金含浸於多孔質碳化矽成形體而成，該鋁-碳化矽質複合體之特徵為：該複合體中碳化矽的比例為60體積%以上，含有60質量%以上75質量%以下之粒徑為80μm以上800μm以下的碳化矽，含有20質量%以上30質量%以下之 粒徑為8μm以上且小於80μm的碳化矽，含有5質量%以上10質量%以下之粒徑為小於8μm的碳化矽。本實施形態中，所謂碳化矽的粒徑係意味著利用電阻試驗方法所算出的粒徑。 The aluminum-silicon carbide composite of this embodiment is formed by impregnating an aluminum alloy with a porous silicon carbide compact. The aluminum-silicon carbide composite is characterized in that the ratio of silicon carbide in the composite is 60 volumes. % Or more, containing 60% by mass or more and 75% by mass or less of silicon carbide having a particle diameter of 80 μm or more and 800 μm or less, and containing 20% by mass or more and 30% by mass or less Silicon carbide having a particle diameter of 8 μm or more and less than 80 μm contains silicon carbide having a particle diameter of less than 8 μm in a range of 5 mass% to 10 mass%. In this embodiment, the particle size of silicon carbide means a particle size calculated by a resistance test method.
[碳化矽質複合體] [Silicon carbide complex]
就本實施形態的鋁-碳化矽質複合體而言，透過將相對於全碳化矽粒子之具有80μm以上且800μm以下的粒徑之粒子的量設為60質量%以上小於75質量%，可顯現230W/mK以上的導熱係數。 The aluminum-silicon carbide composite of the present embodiment can be visualized by setting the amount of particles having a particle diameter of 80 μm or more and 800 μm or less to 60% by mass to 75% by mass relative to the total silicon carbide particles. Thermal conductivity above 230W / mK.
由於前述粒徑為80μm以上，所以變得易於獲得目標的230W/mK以上的導熱係數。又，當小於55質量%時，即使加大複合體中碳化矽含量本身，也無法達成本發明之目的。 Since the aforementioned particle diameter is 80 μm or more, it becomes easy to obtain a target thermal conductivity of 230 W / mK or more. When the content is less than 55% by mass, even if the content of silicon carbide in the composite itself is increased, the object of the invention cannot be achieved.
就本實施形態的鋁-碳化矽質複合體而言，透過將相對於全碳化矽粒子之具有8μm以上且小於80μm的粒徑之粒子的量設為20質量%以上小於30質量%，可獲得能抑制導熱係數降低之效果。 The aluminum-silicon carbide composite of this embodiment can be obtained by setting the amount of particles having a particle diameter of 8 μm or more and less than 80 μm to 20% by mass or less and 30% by mass or less with respect to the total silicon carbide particles. The effect of reducing the thermal conductivity can be suppressed.
又，就本實施形態的鋁-碳化矽質複合體而言，透過將相對於全碳化矽粒子之具有小於8μm的粒徑之粒子的量設為5質量%以上小於10質量%，變得容易獲得目標的7.0ppm/K以下的熱膨脹係數。 In addition, in the aluminum-silicon carbide composite of the present embodiment, it is easy to make the amount of particles having a particle diameter smaller than 8 μm with respect to the total silicon carbide particles to be 5 mass% or more and less than 10 mass%, thereby making it easy. A target thermal expansion coefficient of 7.0 ppm / K or less was obtained.
就本實施形態的鋁-碳化矽質複合體而言，構成該複合體之碳化矽粒子的粒徑及碳化矽的含量係支配大導熱係數的重要因素，其乃基於以下的知識見解，即，在碳化矽粒子具有特定範圍的粒徑且該複合體中碳化 矽含量為特定量以上時，可獲得在室溫(25℃)下具有230W/mK以上的高導熱係數的碳化矽質複合體。 With regard to the aluminum-silicon carbide composite according to this embodiment, the particle size and silicon carbide content of the silicon carbide particles constituting the composite are important factors that govern a large thermal conductivity, which are based on the following knowledge and insights, namely, Silicon carbide particles have a specific range of particle size and are carbonized in the composite When the silicon content is a specific amount or more, a silicon carbide composite having a high thermal conductivity of 230 W / mK or more at room temperature (25 ° C) can be obtained.
又，僅使用粒徑大的碳化矽粉末所獲得之碳化矽質複合體，係因為所使用之碳化矽粒子本身的粒徑大的緣故而少有氧自原料混入，且氧難以透過複合體的製程而受到氧化等之影響混入，所以是具有較高的導熱係數者，但難以顯現230W/mK以上的高導熱係數，其理由是基於以下的知識見解：由於粒徑大的緣故而難以提升複合體中碳化矽含量，再者，就用以提升碳化矽含量所添加之粒徑小的碳化矽粉末而言，其量若未限定在特定範圍則在室溫下無法顯現230W/mK以上的高導熱係數。 In addition, the silicon carbide composite obtained by using only silicon carbide powder having a large particle size has a small particle size due to the large particle size of the silicon carbide particles used, and therefore, little oxygen is mixed in from the raw material, and oxygen is difficult to permeate the composite. It is mixed by the influence of oxidation and the like during the process, so it has a high thermal conductivity, but it is difficult to show a high thermal conductivity above 230W / mK. The reason is based on the following knowledge: it is difficult to improve the composition due to the large particle size. The content of silicon carbide in the body, and for silicon carbide powder with a small particle size added to increase the content of silicon carbide, if the amount is not limited to a specific range, a high temperature of 230 W / mK or more cannot be exhibited at room temperature. Thermal Conductivity.
[鋁合金] [Aluminum alloy]
本實施形態中，在鋁合金方面，可舉出在製作碳化矽質複合體時通常所用的含矽鋁合金、含有矽和鎂的鋁合金以及含鎂鋁合金。當中，從熔融金屬的熔點低且作業性佳方面考量，宜選擇含有矽和鎂的鋁合金，又，從提升所獲得之複合體的導熱係數方面考量，宜選擇含鎂鋁合金。 In this embodiment, examples of the aluminum alloy include a silicon-containing aluminum alloy, a silicon- and magnesium-containing aluminum alloy, and a magnesium-containing aluminum alloy that are generally used when producing a silicon carbide composite. Among them, from the viewpoint of low melting point of molten metal and good workability, an aluminum alloy containing silicon and magnesium should be selected, and from the aspect of improving the thermal conductivity of the obtained composite, a magnesium-containing aluminum alloy should be selected.
為抑制導熱係數的降低，可將矽的含量設為18質量%以下。更佳為，矽的含量是10質量%~14質量%。 In order to suppress a decrease in the thermal conductivity, the content of silicon may be set to 18% by mass or less. More preferably, the content of silicon is from 10% by mass to 14% by mass.
又，針對鎂的含量，經考慮因合金的熔點降低而作業性變好、成為所獲得之複合體的導熱係數降低的原因等，鎂的含量以0.5質量%以上2.5質量%以下較佳。 In addition, considering the content of magnesium, it is considered that the workability is improved due to the lowering of the melting point of the alloy, and the thermal conductivity of the obtained composite is lowered. The content of magnesium is preferably 0.5% by mass or more and 2.5% by mass or less.
再者，0.5質量%以上1.6質量%以下時在25℃的導熱係數為230W/mK以上，1.6質量%以上2.5質量%以下時在 25℃的導熱係數為240W/mK以上，因而更佳。 In addition, the thermal conductivity at 25 ° C. is 230 W / mK or more at 0.5 mass% to 1.6 mass%, and at 1.6 mass% to 2.5 mass%. The thermal conductivity at 25 ° C is more than 240 W / mK, so it is better.
本實施形態的鋁-碳化矽質複合體之用途並不受限定，特別是於如半導體模組用放熱板之被要求更低熱膨脹性的用途中，係以該複合體中碳化矽含量多為理想。因此，較佳為將該複合體中碳化矽含量設為60體積%以上，如此之情形，可獲得在25℃到150℃的複合體之熱膨脹係數為7.0ppm/K以下的複合體。 The use of the aluminum-silicon carbide composite according to this embodiment is not limited, especially in applications requiring lower thermal expansion properties, such as heat sinks for semiconductor modules, where the silicon carbide content in the composite is mostly ideal. Therefore, it is preferable to set the silicon carbide content in the composite to 60% by volume or more. In this case, a composite having a thermal expansion coefficient of 7.0 ppm / K or less at 25 ° C to 150 ° C can be obtained.
[製造方法] [Production method]
在製作本實施形態的鋁-碳化矽質複合體時，只要是使用全碳化矽粒子中具有80μm以上且800μm以下的粒徑之粒子為60質量%以上75質量%以下、具有8μm以上且小於80μm的粒徑之粒子為20質量%以上30質量%以下、及具有小於8μm的粒徑之粒子為5質量%以上10質量%以下所構成的碳化矽粉末而獲得碳化矽的填充度(或相對密度)為60體積%以上的多孔質成形體，並應用以往公知的含浸方法將鋁合金含浸於該多孔質成形體即可。 In the production of the aluminum-silicon carbide composite according to this embodiment, as long as the particles having a particle diameter of 80 μm or more and 800 μm or less among the total silicon carbide particles are used, the particle size is 60% by mass or more and 75% by mass or less, and 8 μm or more and less than 80 μm. A silicon carbide powder having a particle size of 20% by mass or more and 30% by mass or less, and a particle having a particle size of less than 8 μm is 5% by mass or more and 10% by mass or less, thereby obtaining the filling degree (or relative density) of silicon carbide ) Is a porous formed body of 60% by volume or more, and an aluminum alloy may be impregnated into the porous formed body by a conventionally known impregnation method.
在前述以往公知的含浸方法方面，已知有在熔融鋁合金中一邊攪拌碳化矽粉末一邊投入既定量的方法、將碳化矽粉末和鋁合金粉末混合並燒結的粉末冶金法、及預先製作包含有碳化矽的預成形物並將熔融鋁合金含浸於其中的熔融金屬鍛造法和印模壓鑄法等。此等當中，從能作成複合體中碳化矽含量多的觀點、及易於獲得緻密的複合體考量，以製作預成形物且將熔融鋁含浸於其中的方法是較佳方法。 Among the conventionally known impregnation methods described above, a method of adding a predetermined amount while stirring silicon carbide powder in a molten aluminum alloy, a powder metallurgy method in which silicon carbide powder and aluminum alloy powder are mixed and sintered, and a method including pre-production including A molten metal forging method, a die casting method, and the like in which a preform of silicon carbide is impregnated with a molten aluminum alloy. Among these, a method of preparing a preform and impregnating molten aluminum into it is a preferable method from the viewpoint of being capable of forming a large amount of silicon carbide in the composite and considering the ease of obtaining a dense composite.
較佳的含浸方法方面可舉出熔融金屬鍛造法 。因為此方法係將預成形物設置於模具內並投入鋁合金後以機械的壓力加壓的方法，作業容易，且例如在空氣中進行預成形物的預熱處理之情況，可以其預熱不會對預成形物引起大的氧化之溫度條件下含浸鋁合金。關於熔融金屬鍛造法下的一般條件方面，在使鋁合金含浸之際的熔融鋁合金溫度為700℃~850℃，在含浸時的壓力方面係30MPa以上。 Examples of preferred impregnation methods include molten metal forging. . Because this method is a method in which a preform is set in a mold and is put into an aluminum alloy and pressurized with mechanical pressure, the operation is easy, and for example, the preheating of the preform in air can be performed without preheating. The aluminum alloy is impregnated at a temperature that causes large oxidation to the preform. Regarding the general conditions under the molten metal forging method, the temperature of the molten aluminum alloy when the aluminum alloy is impregnated is 700 ° C. to 850 ° C., and the pressure during the impregnation is 30 MPa or more.
以下，在製造本實施形態的鋁-碳化矽質複合體的方法方面，特別透過將鋁合金含浸於預成形物的方法，就本發明作更詳細地說明。 Hereinafter, the present invention will be described in more detail by a method of impregnating an aluminum alloy with a preform in terms of a method for producing the aluminum-silicon carbide composite according to this embodiment.
於製作預成形物之際，在其成形方法方面，可採用模壓成形法、鑄塑成形法、擠製成形法等之公知的成形法，同時可應用以往公知的乾燥、燒結等之處理。又，在進行成形時，使用甲基纖維素、PVA等之有機接合劑或膠態氧化矽、氧化鋁溶膠等之無機接合劑、甚至是作為溶媒的水或有機溶劑等都没有任何問題。 In the production of the preform, a known molding method such as a compression molding method, a cast molding method, an extrusion molding method, or the like can be used for the molding method, and conventionally known processes such as drying and sintering can also be applied. In addition, there is no problem in using an organic bonding agent such as methyl cellulose, PVA, or the like, or an inorganic bonding agent such as colloidal silica or alumina sol, or even water or an organic solvent as a solvent.
即便是施以這樣的各種處理，只要即將進行含浸前的預成形物係為以下之構成即可：由全碳化矽粒子中具有80μm以上且800μm以下的粒徑之粒子為60質量%以上75質量%以下、具有8μm以上且小於80μm的粒徑之粒子為20質量%以上30質量%以下、及具有小於8μm的粒徑之粒子為5質量%以上10質量%以下所構成，且保持碳化矽的填充度為60體積%以上。 Even if such various treatments are performed, the pre-formed system immediately before the impregnation may have the following structure: 60% by mass or more and 75% or less of the particles having a particle diameter of 80 μm or more and 800 μm or less among the total silicon carbide particles % Or less, particles having a particle size of 8 μm or more and less than 80 μm are composed of 20% by mass or more and 30% by mass or less, and particles having a particle size of less than 8 μm are composed of 5% or more and 10% by mass or less, The degree of filling is 60% by volume or more.
預成形物，為了達成顯現其強度之目的，會進行膠態氧化矽或氧化鋁溶膠等之無機接合劑添加，但 此等接合劑係作用於使導熱係數降低的方向。因此，在進行其添加時，應配合在預成形物製作時所使用的碳化矽粉末的粒徑及由其可獲得之預成形物的碳化矽填充度而適宜地調整其添加量。在前述無機接合劑中膠態氧化矽是透過燒結而成為氧化矽和碳化矽粒子結合並顯現出足夠的預成形物強度，故為較佳者，但會因此等無機接合劑之添加而導致來自於無機接合劑之氧增量，故應限制其添加量。 In order to achieve the strength of the preform, an inorganic bonding agent such as colloidal silica or alumina sol is added, but These bonding agents act in a direction that decreases the thermal conductivity. Therefore, the addition amount should be adjusted appropriately in accordance with the particle size of the silicon carbide powder used in the preparation of the preform and the silicon carbide filling degree of the preform obtained from the preform. In the aforementioned inorganic bonding agent, colloidal silicon oxide is sintered to become a combination of silicon oxide and silicon carbide particles, and exhibits sufficient strength of the preform. Therefore, it is preferable, but it will be caused by the addition of the inorganic bonding agent. The amount of oxygen added to the inorganic bonding agent should be limited.
在製作本實施形態的鋁-碳化矽質複合體時，在例如固體成分濃度為20質量%的氧化矽溶膠的情況，無機接合劑的添加量係以相對於全碳化矽粒子是10質量%以下者為宜。就無機接合劑的添加量為10質量%以上而言在25℃的導熱係數為230W/mK以上，就10質量%以上而言，在25℃的導熱係數為245W/mK以上。 When producing the aluminum-silicon carbide composite according to this embodiment, for example, in the case of a silica sol having a solid content concentration of 20% by mass, the addition amount of the inorganic bonding agent is 10% by mass or less relative to the total silicon carbide particles. It is better. The thermal conductivity at 25 ° C. is 230 W / mK or more when the additive amount of the inorganic bonding agent is 10% by mass or more, and the thermal conductivity at 25 ° C. is 245 W / mK or more.
預成形物，為了達成利用前述無機接合劑使顯現強度等之目的，一般會進行燒結。此際，通常是在空氣中等氧環境氣體進行燒結，但會有構成預成形物的碳化矽粉末因為該燒結而稍被氧化，成為在複合體中導熱係數降低的原因之情形。因此，在進行預成形物的燒結時，應因應於所使用的碳化矽粉末的粒徑，採用盡可能不易氧化的條件。例如，在空氣中的燒結雖亦取決於其保持時間，但以在小於950℃的溫度下進行而得以盡可能抑制氧化者為宜。較佳的溫度範圍方面係750℃~900℃。又，在非氧化性的環境氣體中之燒結方法方面，可舉出在氬、氦、氫、氮等之非氧化性氣體中或真空中 進行燒結的方法。 The preform is generally sintered for the purpose of developing the strength and the like using the inorganic bonding agent. At this time, the sintering is usually performed in an oxygen ambient gas such as air, but the silicon carbide powder constituting the preform may be slightly oxidized due to the sintering, which may cause the thermal conductivity of the composite to decrease. Therefore, when the sintering of the preform is performed, it is necessary to adopt conditions that are not as easy to be oxidized as possible in accordance with the particle diameter of the silicon carbide powder used. For example, although sintering in air also depends on its holding time, it is preferable to perform the sintering in air at a temperature of less than 950 ° C to suppress oxidation as much as possible. The preferred temperature range is 750 ° C to 900 ° C. In addition, as for the sintering method in a non-oxidizing ambient gas, a non-oxidizing gas such as argon, helium, hydrogen, nitrogen or the like can be mentioned. Method of sintering.
又，在將鋁合金含浸於預成形物的方法方面，可使用熔融金屬鍛造法、印模壓鑄法及其等改良的方法等公知的方法。此外，在含浸時，通常其預備步驟方面一般是進行預成形物的預熱處理，俾使鋁合金可容易浸透。關於預熱處理，需留意當用以構成預成形物的碳化矽粒子被氧化時其氧量應不超過1.4質量%，再者，氧量宜抑制在1.1質量%以下。 As a method of impregnating an aluminum alloy with a preform, a known method such as a molten metal forging method, a die-casting method, and other improved methods can be used. In addition, during the impregnation, the pre-processing of the preform is generally performed in the preparatory steps, so that the aluminum alloy can be easily impregnated. Regarding the pre-heat treatment, it should be noted that when the silicon carbide particles used to constitute the preform are oxidized, the amount of oxygen should not exceed 1.4% by mass, and the amount of oxygen should be suppressed to 1.1% by mass or less.
上述實施形態的鋁-碳化矽質複合體由於具有230W/mK以上的高導熱係數，所以適合於電源模組用的散熱材。又，因為在25℃到150℃中之熱膨脹係數為7.0ppm/K以下，故可用作為半導體模組用放熱板。 Since the aluminum-silicon carbide composite according to the above embodiment has a high thermal conductivity of 230 W / mK or more, it is suitable for a heat sink for a power module. In addition, since the thermal expansion coefficient at 25 ° C to 150 ° C is 7.0 ppm / K or less, it can be used as a heat sink for a semiconductor module.
又，上述實施形態的鋁-碳化矽質複合體係其比重約為3左右的低比重，且在作為汽車、電車等之移動裝置用的搭載材料方面亦有幫助。 In addition, the aluminum-silicon carbide composite system of the above embodiment has a low specific gravity of about 3, and is also useful as a mounting material for mobile devices such as automobiles and trams.
[實施例1] [Example 1]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末65質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末25質量%、具有小於8μm的粒徑之碳化矽粉末10質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)8.9質量%、水12質量%，將此等混合而調整漿液。使此漿液流進石膏模並放置，之後經脫模、乾燥而獲得成形體。此成形體在空氣中以1000℃進行4小時燒結作成預成形物。 65% by mass of silicon carbide powder having a particle size of 80 μm or more and 800 μm or less, 25% by mass of silicon carbide powder having a particle size of 8 μm or more and less than 80 μm, 10% by mass of silicon carbide powder having a particle size less than 8 μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 8.9% by mass and 12% by mass of water, and these were mixed to adjust the slurry. This slurry was poured into a gypsum mold and left to stand, and then the mold was demolded and dried to obtain a formed body. This formed body was sintered in air at 1000 ° C for 4 hours to prepare a preform.
在具有80μm以上且800μm以下的粒徑之碳化矽粉末方面，使用了太平洋藍登光器件有限公司製NG-F80。 For the silicon carbide powder having a particle diameter of 80 μm or more and 800 μm or less, NG-F80 manufactured by Pacific Blue Board Optical Devices Co., Ltd. was used.
又，以具有8μm以上且小於80μm的粒徑之碳化矽粉末成為25質量%、具有小於8μm的粒徑之碳化矽粉末成為10質量%的方式，使用將南興陶瓷公司製GC-# 500、屋久島電工公司製GC-1000F及南興陶瓷公司製GC-# 4000以13.5：16.5：5.0的摻合率混合的粉末。 In addition, GC- # 500 manufactured by Nanxing Ceramics Co., Ltd. was used so that the silicon carbide powder having a particle diameter of 8 μm or more and less than 80 μm became 25% by mass and the silicon carbide powder having a particle diameter of less than 8 μm became 10% by mass. GC-1000F manufactured by Yakushima Electric Works Co., Ltd. and GC- # 4000 manufactured by Nanxing Ceramics Co., Ltd. were mixed at a blending ratio of 13.5: 16.5: 5.0.
針對前述預成形物的一部份，為測定密度而加工成直徑50mm、厚度5mm。預成形物之碳化矽的填充度係69.6%。預成形物之碳化矽填充度，係以碳化矽的理論密度3.21g/cm3除上述加工品的密度，用百分率來定義。 A part of the preform was processed into a diameter of 50 mm and a thickness of 5 mm in order to measure the density. The pre-formed silicon carbide has a filling degree of 69.6%. The silicon carbide filling degree of the preform is defined by dividing the density of the processed product by the theoretical density of silicon carbide of 3.21 g / cm 3 and using the percentage.
針對剩餘的預成形物，藉由在空氣中650℃進行1小時燒結而進行了預熱處理。在預熱後馬上將預成形物設置於模具內，之後，將含有矽12質量%、鎂1質量%的在850℃下熔融的鋁合金以預成形物的前面被十分遮蔽的方式投入模具內。之後，快速地利用沖頭以56MPa的壓力按壓14分鐘，冷卻後，從模具內將含有碳化矽質複合體的鋁合金塊取出。再由此塊將碳化矽質複合體切出。 The remaining preforms were preheated by sintering in air at 650 ° C for 1 hour. Immediately after preheating, the preform was set in a mold, and then an aluminum alloy melted at 850 ° C containing 12% by mass of silicon and 1% by mass of magnesium was put into the mold so that the front surface of the preform was completely shielded. . Thereafter, the punch was quickly pressed at a pressure of 56 MPa for 14 minutes using a punch, and after cooling, the aluminum alloy block containing the silicon carbide composite was taken out from the mold. Then cut out the silicon carbide composite from this block.
為測定前述複合體在室溫的導熱係數，將一部份加工成縱25mm、橫25mm、厚度1mm作為試料。經以雷射閃光法測定此試料的導熱係數之結果，其導熱係數為252W/mK。針對熱膨脹係數測定用試料，從前述複合體將既定形狀的試料切出，測定從室溫(25℃)到150℃為止的熱膨脹係數。此結果顯示在表1。 In order to measure the thermal conductivity of the composite at room temperature, a part was processed into 25 mm in length, 25 mm in width, and 1 mm in thickness as samples. As a result of measuring the thermal conductivity of this sample by a laser flash method, the thermal conductivity was 252 W / mK. Regarding the sample for measuring the coefficient of thermal expansion, a sample having a predetermined shape was cut out from the composite, and the coefficient of thermal expansion from room temperature (25 ° C) to 150 ° C was measured. This result is shown in Table 1.
[實施例2] [Example 2]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末65質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末26質量%、具有小於8μm的粒徑之碳化矽粉末9質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)11.6質量%、水9質量%，將此等混合而調整漿液。 65% by mass of silicon carbide powder having a particle size of 80 μm or more and 800 μm or less, 26% by mass of silicon carbide powder having a particle size of 8 μm or more and less than 80 μm, 9% by mass of silicon carbide powder having a particle size less than 8 μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 11.6% by mass and 9% by mass of water. These are mixed to adjust the slurry.
在具有80μm以上且800μm以下的粒徑之碳化矽粉末方面，使用了太平洋藍登光器件有限公司製NG-F80。 For the silicon carbide powder having a particle diameter of 80 μm or more and 800 μm or less, NG-F80 manufactured by Pacific Blue Board Optical Devices Co., Ltd. was used.
又，以具有8μm以上且小於80μm的粒徑之碳化矽粉末成為26質量%、具有小於8μm的粒徑之碳化矽粉末成為9質量%的方式，使用將南興陶瓷公司製GC-# 500、屋久島電工公司製GC-1000F及GMF-4S以13.5：16.5：5.0的摻合率混合的粉末。 In addition, GC- # 500 manufactured by Nanxing Ceramics Co., Ltd. was used so that the silicon carbide powder having a particle diameter of 8 μm or more and less than 80 μm became 26% by mass, and the silicon carbide powder having a particle diameter of less than 8 μm was 9% by mass. GC-1000F and GMF-4S manufactured by Yakushima Electric Co., Ltd. are powders mixed at a blending ratio of 13.5: 16.5: 5.0.
以和實施例1相同的方法製作預成形物及複合體。結果顯示在表1。 A preform and a composite were produced in the same manner as in Example 1. The results are shown in Table 1.
[實施例3] [Example 3]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末65質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末25質量%、具有小於8μm的粒徑之碳化矽粉末10質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)12.0質量%、水9質量%，將此等混合而調整漿液。 65% by mass of silicon carbide powder having a particle size of 80 μm or more and 800 μm or less, 25% by mass of silicon carbide powder having a particle size of 8 μm or more and less than 80 μm, 10% by mass of silicon carbide powder having a particle size less than 8 μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 12.0% by mass and 9% by mass of water, and these are mixed to adjust the slurry.
在具有80μm以上且800μm以下的粒徑之碳化 矽粉末方面，使用了太平洋藍登光器件有限公司製NG-F80。 Carbonization with a particle size of 80 μm or more and 800 μm or less For the silicon powder, NG-F80 manufactured by Pacific Landon Optical Devices Co., Ltd. was used.
又，以具有8μm以上且小於80μm的粒徑之碳化矽粉末成為25質量%、具有小於8μm的粒徑之碳化矽粉末成為10質量%的方式，使用將南興陶瓷公司製GC-# 500、屋久島電工公司製GC-1000F及南興陶瓷公司製GC-# 4000以13.5：16.5：5.0的摻合率混合的粉末。以和實施例1相同的方法製作預成形物。 In addition, GC- # 500 manufactured by Nanxing Ceramics Co., Ltd. was used so that the silicon carbide powder having a particle diameter of 8 μm or more and less than 80 μm became 25% by mass and the silicon carbide powder having a particle diameter of less than 8 μm became 10% by mass. GC-1000F manufactured by Yakushima Electric Works Co., Ltd. and GC- # 4000 manufactured by Nanxing Ceramics Co., Ltd. were mixed at a blending ratio of 13.5: 16.5: 5.0. A preform was produced in the same manner as in Example 1.
使用鋁合金是含有矽12質量%、鎂0.9質量%的鋁合金製作了複合體。結果顯示在表1。 A composite was produced using an aluminum alloy containing 12% by mass of silicon and 0.9% by mass of magnesium. The results are shown in Table 1.
[實施例4] [Example 4]
除了設成含有矽12質量%之鋁合金，含有鎂1.2質量%之鋁合金不同以外，其餘同實施例3的方法製作預成形物及複合體。結果顯示在表1。 Except that the aluminum alloy containing 12% by mass of silicon and the aluminum alloy containing 1.2% by mass of magnesium were different, the preforms and composites were produced in the same manner as in Example 3. The results are shown in Table 1.
[實施例5] [Example 5]
除了設成含有矽12質量%之鋁合金，含有鎂1.6質量%之鋁合金不同以外，其餘同實施例3的方法製作預成形物及複合體。結果顯示在表1。 Except that the aluminum alloy containing 12% by mass of silicon and the aluminum alloy containing 1.6% by mass of magnesium were different, the preforms and composites were produced in the same manner as in Example 3. The results are shown in Table 1.
[實施例6] [Example 6]
在具有80μm以上且800μm以下的粒徑之碳化矽粉末方面，使用了太平洋藍登光器件有限公司製NG-F80。 For the silicon carbide powder having a particle diameter of 80 μm or more and 800 μm or less, NG-F80 manufactured by Pacific Blue Board Optical Devices Co., Ltd. was used.
又，以具有8μm以上且小於80μm的粒徑之碳化矽粉末成為25質量%、具有小於8μm的粒徑之碳化矽粉末成為10質量%的方式，使用將南興陶瓷公司製GC-# 500、屋久島電工公司製GC-1000F及南興陶瓷公司製GC-# 6000 以13.5：16.5：5.0的摻合率混合的粉末。 In addition, GC- # 500 manufactured by Nanxing Ceramics Co., Ltd. was used so that the silicon carbide powder having a particle diameter of 8 μm or more and less than 80 μm became 25% by mass and the silicon carbide powder having a particle diameter of less than 8 μm became 10% by mass. GC-1000F made by Yakushima Electric Works and GC- # 6000 made by Nanxing Ceramics The powder was mixed at a blending ratio of 13.5: 16.5: 5.0.
除了秤取6質量%之膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)而調整漿液這點不同以外，其餘同實施例3的方法製作預成形物及複合體。結果顯示在表1。 Except for weighing 6% by mass of colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industry Co., Ltd., containing 20% by mass of solids) and adjusting the slurry, the other methods were the same as those in Example 3 to make preforms and composites. . The results are shown in Table 1.
[實施例7] [Example 7]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末60質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末30質量%、具有小於8μm的粒徑之碳化矽粉末10質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)12質量%、水9質量%，將此等混合而調整漿液。 60% by mass of silicon carbide powder having a particle size of 80 μm or more and 800 μm or less, 30% by mass of silicon carbide powder having a particle size of 8 μm or more and less than 80 μm, 10% by mass of silicon carbide powder having a particle size of less than 8 μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 12% by mass and 9% by mass of water. These are mixed to adjust the slurry.
以具有80μm以上且800μm以下的粒徑之碳化矽粉末成為60質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末成為30質量%、具有小於8μm的粒徑之碳化矽粉末成為10質量%的方式，使用將太平洋藍登光器件有限公司製NG-F54、太平洋藍登光器件有限公司製GC-# 500及太平洋藍登光器件有限公司製GC-# 3000以60：30：10的摻合率混合的粉末。 The silicon carbide powder having a particle size of 80 μm or more and 800 μm or less becomes 60% by mass, the silicon carbide powder having a particle size of 8 μm or more and less than 80 μm becomes 30% by mass, and the silicon carbide powder having a particle size of less than 8 μm becomes 10 mass % Method, using NG-F54 manufactured by Pacific Landon Optical Devices Co., Ltd., GC- # 500 manufactured by Pacific Blue Board Optical Devices Co., Ltd. and GC- # 3000 manufactured by Pacific Blue Board Optical Devices Co., Ltd. at 60:30:10. Blend rate mixed powder.
以和實施例1相同的方法製作預成形物及複合體。結果顯示在表1。 A preform and a composite were produced in the same manner as in Example 1. The results are shown in Table 1.
[實施例8] [Example 8]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末75質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末25質量%、具有小於8μm的粒徑之碳化矽粉末5質量 %及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)12質量%、水9質量%，將此等混合而調整漿液。 Weigh 75 mass% of silicon carbide powder with a particle size of 80 μm or more and 800 μm or less, 25 mass% of silicon carbide powder with a particle size of 8 μm or more and less than 80 μm, and 5 mass of silicon carbide powder with a particle size of less than 8 μm. % And colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 12% by mass and 9% by mass of water. These are mixed to adjust the slurry.
以具有80μm以上且800μm以下的粒徑之碳化矽粉末成為75質量%，具有8μm以上且小於80μm的粒徑之碳化矽粉末成為20質量%、具有小於8μm的粒徑之碳化矽粉末成為5質量%的方式，使用將太平洋藍登光器件有限公司製NG-F30、太平洋藍登光器件有限公司製NG-F220及太平洋藍登光器件有限公司製GC-# 2000以60：30：10的摻合率混合的粉末。 The silicon carbide powder having a particle size of 80 μm or more and 800 μm or less becomes 75% by mass, the silicon carbide powder having a particle size of 8 μm or more and less than 80 μm becomes 20% by mass, and the silicon carbide powder having a particle size of less than 8 μm becomes 5 mass % Method, using 60:30:10 blending of NG-F30 made by Pacific Landon Optical Device Co., Ltd., NG-F220 made by Pacific Landon Optical Device Co., Ltd. and GC- # 2000 made by Pacific Landon Optical Device Co., Ltd. Mixing powder.
以和實施例3相同的方法製作預成形物及複合體。結果顯示在表1。 A preform and a composite were produced in the same manner as in Example 3. The results are shown in Table 1.
[實施例9] [Example 9]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末70質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末20質量%、具有小於8μm的粒徑之碳化矽粉末10質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)12質量%、水9質量%，將此等混合而調整漿液。 Weigh 70% by mass of silicon carbide powder with a particle size of 80 μm or more and 800μm or less, 20% by mass of silicon carbide powder with a particle size of 8μm or more and less than 80μm, 10% by mass of silicon carbide powder with a particle size less than 8μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 12% by mass and 9% by mass of water. These are mixed to adjust the slurry.
在具有80μm以上且800μm以下的粒徑之碳化矽粉末，使用了太平洋藍登光器件有限公司製NG-F80。 For the silicon carbide powder having a particle diameter of 80 μm or more and 800 μm or less, NG-F80 manufactured by Pacific Blue Board Optical Devices Co., Ltd. was used.
又，以具有8μm以上且小於80μm的粒徑之碳化矽粉末成為20質量%、具有小於8μm的粒徑之碳化矽粉末成為10質量%的方式，將太平洋藍登光器件有限公司製GC-# 800及太平洋藍登光器件有限公司製GC-# 6000以20： 10的摻合率混合。 In addition, GC- # made by Pacific Landon Optical Co., Ltd. was made so that the silicon carbide powder having a particle diameter of 8 μm or more and less than 80 μm became 20% by mass and the silicon carbide powder having a particle diameter of less than 8 μm became 10% by mass. 800 and Pacific Landon Optical Device Co., Ltd. GC- # 6000 to 20: A blending ratio of 10 was mixed.
以和實施例1相同的方法製作預成形物及複合體。鋁合金係為矽12質量%且鎂1.6質量%者。 A preform and a composite were produced in the same manner as in Example 1. The aluminum alloy is 12% by mass of silicon and 1.6% by mass of magnesium.
[實施例10] [Example 10]
除了設成含有矽12質量%之鋁合金，含有鎂2.1質量%之鋁合金不同以外，其餘同實施例9的方法製作預成形物及複合體。 Except that the aluminum alloy containing 12% by mass of silicon and the aluminum alloy containing 2.1% by mass of magnesium were different, the preforms and composites were produced in the same manner as in Example 9.
[比較例] [Comparative example]
秤取具有80μm以上且800μm以下的粒徑之碳化矽粉末55質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末40質量%、具有小於8μm的粒徑之碳化矽粉末5質量%及膠態氧化矽(日產化學工業公司製SNOWTEX O，含有20質量%之固體物)12質量%、水12質量%，將此等混合而調整漿液。使此漿液流進石膏模並放置，之後經脫模、乾燥而獲得成形體。此成形體在空氣中以1000℃進行4小時燒結作成預成形物。 55% by mass of silicon carbide powder having a particle size of 80 μm or more and 800 μm or less, 40% by mass of silicon carbide powder having a particle size of 8 μm or more and less than 80 μm, 5% by mass of silicon carbide powder having a particle size of less than 8 μm, and Colloidal silica (SNOWTEX O manufactured by Nissan Chemical Industries, Inc., containing 20% by mass of solids) 12% by mass and 12% by mass of water. These are mixed to adjust the slurry. This slurry was poured into a gypsum mold and left to stand, and then the mold was demolded and dried to obtain a formed body. This formed body was sintered in air at 1000 ° C for 4 hours to prepare a preform.
以具有80μm以上且800μm以下的粒徑之碳化矽粉末成為55質量%、具有8μm以上且小於80μm的粒徑之碳化矽粉末成為40質量%、具有小於8μm的粒徑之碳化矽粉末成為5質量%的方式，使用將太平洋藍登光器件有限公司製NG-F150及屋久島電工公司製GC-1000F以2：1的摻合率混合的粉末。 The silicon carbide powder having a particle size of 80 μm or more and 800 μm or less becomes 55 mass%, the silicon carbide powder having a particle size of 8 μm or more and less than 80 μm becomes 40 mass%, and the silicon carbide powder having a particle size of less than 8 μm becomes 5 mass In the method of%, a powder obtained by mixing NG-F150 manufactured by Pacific Blue Light Co., Ltd. and GC-1000F manufactured by Yakushima Electric Co., Ltd. at a mixing ratio of 2: 1 was used.
從表1可知，本發明的實施例1至10的鋁-碳化矽質複合體具有高的導熱且具有低的熱膨脹係數。且可知此等鋁-碳化矽質複合體係低比重。 As can be seen from Table 1, the aluminum-silicon carbide composites of Examples 1 to 10 of the present invention have high thermal conductivity and low coefficient of thermal expansion. It is also known that these aluminum-silicon carbide composite systems have a low specific gravity.
如上所述，本發明的鋁-碳化矽質複合體由於具有高導熱係數，所以適合作為電源模組用的散熱材，且由於具有低的熱膨脹係數，故可用作為半導體模組用放熱板。又，因為其比重低，故在作為汽車、電車等之移動裝置用的搭載材料方面亦有幫助。 As described above, the aluminum-silicon carbide composite of the present invention is suitable as a heat sink for a power module because of its high thermal conductivity, and because it has a low thermal expansion coefficient, it can be used as a heat sink for a semiconductor module. In addition, because of its low specific gravity, it is also useful as a mounting material for mobile devices such as automobiles and trams.
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