TW202100453A - Method of directly producing spherical aluminum nitride from aluminum metal - Google Patents
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本發明係有關於一種製造方法,特別是一種鋁金屬直接製作球型氮化鋁之方法。The invention relates to a manufacturing method, in particular to a method for directly manufacturing spherical aluminum nitride from aluminum metal.
氮化鋁其因具有高傳導率,低的介電長度損失,良好的電絕緣性等特性因素,故氮化鋁於電子應用材料中是屬於非常熱門的一種原材料,其可應用的範圍非常的廣泛,例如可應用於半導體與微電子封裝基板、高亮度LED晶片乘載基板、車用電子與照明元件、高功率電子元件散熱材料等方面,是未來具有潛力的材料之一。Aluminum nitride has high conductivity, low dielectric length loss, good electrical insulation and other characteristics, so aluminum nitride is a very popular raw material in electronic application materials, and its applicable range is very wide. It can be widely used in semiconductor and microelectronic packaging substrates, high-brightness LED chip carrier substrates, automotive electronics and lighting components, and high-power electronic components heat dissipation materials. It is one of the potential materials in the future.
查,關於習知氮化鋁粉末合成方法非常多,例如舉例習知製作方式進行,其依序採取下列步驟: (1) 利用r-氧化鋁和碳粉混合,置入高溫氣氛燒結爐燒結,燒結溫度攝氏溫度1400度左右,製得氮化鋁粉。 (2) 利用防爆造粒機,再次造粒至所需尺寸,且其同時該造粒所得之表面尚附著碳粉。 (3) 再次置入高溫氣氛燒結爐燒結,燒結溫度攝氏溫度1850度左右,以製得氮化鋁粉。 (4) 置入低溫大氣爐除碳,因其表面碳的結層不均勻,易燒結出的氮化鋁成塊狀。 (5) 利用粉碎機將塊狀的氮化鋁粉碎,再依篩選機篩選所需粒徑,粉碎後氮化鋁粉,所製得氮化鋁粉是異行(圖1)。 (6) 將第六項異行氮化鋁粉,置入攝氏溫度2300度的等離子機修飾氮化鋁粉表面至90%真圓。Check, there are many conventional methods for the synthesis of aluminum nitride powder, for example, the conventional production method is used, and the following steps are taken in order: (1) Use r-alumina and carbon powder to mix, put in a high-temperature atmosphere sintering furnace for sintering, and the sintering temperature is about 1400 degrees Celsius to prepare aluminum nitride powder. (2) Using an explosion-proof granulator, granulate again to the required size, and at the same time, the surface obtained by the granulation still adheres to carbon powder. (3) Put it into a high-temperature atmosphere sintering furnace again for sintering, and the sintering temperature is about 1850 degrees Celsius to obtain aluminum nitride powder. (4) Put it into a low-temperature atmospheric furnace to remove carbon. Because of the uneven carbon layer on the surface, the aluminum nitride that is easily sintered becomes a block. (5) Use a pulverizer to crush the massive aluminum nitride, and then screen the required particle size according to the sieving machine. After crushing the aluminum nitride powder, the aluminum nitride powder obtained is different (Figure 1). (6) Put the sixth different aluminum nitride powder into a plasma machine with a temperature of 2300 degrees Celsius to modify the surface of the aluminum nitride powder to 90% true circle.
然,上述有關該氮化鋁之製作方法並不能夠大量生產,其主要在於該等氮化鋁成型後,並非呈現出所需之圓球顆粒狀態,再加上該等氮化鋁製作過程易產生相互連結,故必須再進行破碎、研磨等作業,再加上該等氮化鋁的顆粒細小,因此在研磨作業中亦必須注意加工速度,以及設備的安全性,否則易產生氣爆危險,故習知生產通常1個小時最多只能生產約5公斤的量而已,所以製作成本高且耗能與耗時,實有待改進。However, the above-mentioned manufacturing method of the aluminum nitride cannot be mass-produced. The main reason is that the aluminum nitride does not show the required spherical particle state after being formed, and the manufacturing process of the aluminum nitride is easy. Because of the mutual connection, crushing and grinding must be carried out. In addition, the particles of aluminum nitride are small. Therefore, the processing speed and the safety of the equipment must be paid attention to during the grinding operation. Otherwise, the risk of gas explosion may occur. Therefore, conventional production can only produce about 5 kilograms in one hour. Therefore, the production cost is high and energy and time consuming, and it needs to be improved.
因此,本發明之目的,是在提供一種鋁金屬直接製作球型氮化鋁,其可達到快速、節能、低成本且可量產的製作出球型氮化鋁。Therefore, the purpose of the present invention is to provide a method of directly manufacturing spherical aluminum nitride from aluminum metal, which can achieve rapid, energy-saving, low-cost and mass-produced manufacturing of spherical aluminum nitride.
於是,本發明鋁金屬直接製作球型氮化鋁,其包含備料步驟、造粒步驟、篩選步驟、混合步驟及燒結步驟;其中,該備料步驟中採用純度80%以上的鋁金屬;另,該造粒步驟係將該鋁金屬熱熔後,經輸入一噴霧造粒機後造粒形成一球型鋁粉;又,該篩選步驟中係利用篩選機篩選出小於200um粒徑以下之球型鋁粉;至於,該混合步驟係備置有一促進劑,以將前述該球型鋁粉與該促進劑,以適當比率進行均勻攪拌混合;最後,該燒結步驟再將該混合物置入高壓氣氛燒結爐,並以攝氏溫度為400度以上,且壓力控制為50公斤以下,使該球型鋁粉末進行轉化反應,形成一球型氮化鋁;是以,透過上述之流程,能大量簡化該球型氮化鋁之製造程序,而製造出所需之球型氮化鋁型態,且此過程中避免不必要的研磨作業進行,有效增加生產速度、降低生產成本外,同時於生產過程中也可以降低所需耗能,進而達到快速、節能、低成本且可量產等目的。Therefore, the aluminum metal of the present invention directly produces spherical aluminum nitride, which includes a material preparation step, a granulation step, a screening step, a mixing step, and a sintering step; wherein, the aluminum metal with a purity of 80% or more is used in the material preparation step; The granulation step is to melt the aluminum metal into a spray granulator and then granulate to form a spherical aluminum powder; in the screening step, a sieving machine is used to screen out spherical aluminum with a particle size of less than 200um As for the mixing step, an accelerator is prepared to uniformly stir and mix the aforementioned spherical aluminum powder and the accelerator at an appropriate ratio; finally, the sintering step puts the mixture into a high-pressure atmosphere sintering furnace, And the temperature is 400 degrees Celsius or more, and the pressure is controlled below 50 kg, so that the spherical aluminum powder undergoes a conversion reaction to form a spherical aluminum nitride; therefore, through the above process, the spherical nitrogen can be greatly simplified The process of manufacturing aluminum, and the required spherical aluminum nitride shape is produced, and unnecessary grinding operations are avoided during this process, which effectively increases the production speed and reduces the production cost. At the same time, the production process can also be reduced Energy consumption is required to achieve rapid, energy-saving, low-cost and mass-produced purposes.
有關本發明之前述及其他技術內容、特點與功效,在以下配合參考圖式之較佳實施例的詳細說明中,將可清楚地明白。The foregoing and other technical content, features, and effects of the present invention will be clearly understood in the following detailed description of the preferred embodiment with reference to the drawings.
參閱圖2,本發明鋁金屬直接製作球型氮化鋁之方法的第一較佳實施例,該方法包含有備料步驟、造粒步驟、篩選步驟、混合步驟及燒結步驟;其中,該備料步驟備置有純度80%重量百分比以上之鋁金屬,該鋁金屬可為鋁錠、鋁屑等等;另,該造粒步驟係將該鋁金屬熱熔後,輸入一造粒機造粒形成一球型鋁粉,而該熱熔溫度至少為攝氏500度以上,以使該鋁金屬可以熱熔形成液狀,而輸入至造粒機進行造粒,而該造粒機,於本實施例中係以噴霧造粒機為例加以說明,而該噴霧造粒機入口氣壓調製適當的公斤壓力範圍,調整適當之壓力及熔液流量大小,以製得各種範圍的鋁粉粒徑。Referring to FIG. 2, the first preferred embodiment of the method for directly manufacturing spherical aluminum nitride from aluminum metal of the present invention includes a preparation step, a granulation step, a screening step, a mixing step, and a sintering step; wherein, the preparation step Prepare aluminum metal with a purity of more than 80% by weight. The aluminum metal can be aluminum ingots, aluminum scraps, etc.; in addition, the pelletizing step is to input the aluminum metal into a pelletizer to pelletize to form a ball Type aluminum powder, and the hot-melting temperature is at least 500 degrees Celsius, so that the aluminum metal can be hot-melted into a liquid state, and then input to the granulator for granulation, and the granulator is in this embodiment Take a spray granulator as an example to illustrate, and the inlet air pressure of the spray granulator is adjusted to an appropriate kilogram pressure range, and the appropriate pressure and melt flow are adjusted to obtain various ranges of aluminum powder particle size.
仍續前述,該篩選步驟係備置有一篩選機,以將該球型鋁粉輸入該篩選機內,以篩選出粒徑小於200um以下之球型鋁粉為之;另,該混合步驟係備置有一促進劑,該促進劑於本實施例中係以疊氮化鈉為例,其將該球型鋁粉與促進劑以比例70%~98%重量百分比 :2%~30%重量百分比均勻混合成一混合物;最後,該燒結步驟係將該混合物置入高壓氣氛燒結爐(圖中未示出),而該高壓氣氛燒結爐之爐體攝氏溫度至少為400度以上,其較佳之範圍為500度~1400度,而該爐體壓力設定可在50公斤以內,較佳為2~40公斤之範圍,使該球型粉末在燒結過程中,除該高壓氣氛燒結爐之爐體達到設定所需溫度時,持溫1~3小時後即可斷電,以使前述置入之該混合物進行轉化反應,形成一球型氮化鋁,而呈圖3所示狀態;因此,透過上述製造方法,其可簡化製造該球型氮化鋁製造步驟,使得生產速度能獲得快速提升,並且可以達到量產之功效外,同時也可以相對降低生產成本及降低所需耗能,進而使該球型氮化鋁之製程兼具有快速、節能、低成本且可量產等功效。Continuing the foregoing, the screening step is equipped with a screening machine to input the spherical aluminum powder into the screening machine to screen out the spherical aluminum powder with a particle size of less than 200um; in addition, the mixing step is equipped with a Accelerator. In this embodiment, sodium azide is used as an example for the accelerator. The spherical aluminum powder and the accelerator are uniformly mixed in a ratio of 70% to 98% by weight: 2% to 30% by weight. Mixture; Finally, the sintering step is to put the mixture into a high-pressure atmosphere sintering furnace (not shown in the figure), and the temperature of the furnace body of the high-pressure atmosphere sintering furnace is at least 400 degrees Celsius, and the preferred range is 500 degrees ~ 1400 degrees, and the furnace body pressure can be set within 50 kg, preferably in the range of 2-40 kg, so that the spherical powder is sintered, except when the furnace body of the high-pressure atmosphere sintering furnace reaches the set required temperature After holding the temperature for 1 to 3 hours, the power can be turned off, so that the previously placed mixture undergoes a conversion reaction to form a spherical aluminum nitride, which is in the state shown in Figure 3. Therefore, through the above manufacturing method, it can be The manufacturing steps of the spherical aluminum nitride are simplified, so that the production speed can be quickly increased, and the effect of mass production can be achieved, while the production cost and the required energy consumption can be relatively reduced, thereby making the spherical aluminum nitride The process has the advantages of fast, energy-saving, low-cost and mass production.
參閱圖4,本發明鋁金屬直接製作球型氮化鋁之方法的第二較佳實施例,其仍包含有備料、造粒、篩選、混合及燒結等步驟,且前述步驟所揭示之要件與欲達成之功效皆與第一實施例相同,恕不詳述,特別是,本實施例中為降低該球型氮化鋁之含氧量特性,更可於該燒結步驟後接續有塗層步驟、高溫燒結步驟及精煉步驟;其中,該塗層步驟係將該球型氮化鋁,利用塗層機將其表面披覆碳粉,而該碳粉可為200奈米以下之碳粉;另,該高溫燒結步驟係將披覆有碳粉之球型氮化鋁置入入高溫氣氛燒結爐燒結,並使該爐溫加熱至少為攝氏溫度 1400 度以上,然後降溫;最後,該精煉步驟係將經前述步驟後之球型氮化鋁置入一高溫氣爐中,並將溫度控制於400~700度範圍內,使該球形氮化鋁進行除碳,將可得到一低含氧量特性之球形氮化鋁。Referring to FIG. 4, the second preferred embodiment of the method for directly manufacturing spherical aluminum nitride from aluminum metal of the present invention still includes the steps of material preparation, granulation, screening, mixing, and sintering, and the requirements disclosed in the foregoing steps and The effects to be achieved are the same as those of the first embodiment and will not be described in detail. In particular, in this embodiment, in order to reduce the oxygen content characteristics of the spherical aluminum nitride, a coating step can be continued after the sintering step. , High-temperature sintering step and refining step; wherein, the coating step is to coat the spherical aluminum nitride surface with carbon powder using a coating machine, and the carbon powder can be carbon powder below 200 nanometers; The high-temperature sintering step is to put the carbon powder-coated spherical aluminum nitride into a high-temperature atmosphere sintering furnace, and heat the furnace to a temperature of at least 1400 degrees Celsius, and then lower the temperature; finally, the refining step is Put the spherical aluminum nitride after the foregoing steps into a high-temperature gas furnace and control the temperature within the range of 400 to 700 degrees to remove carbon from the spherical aluminum nitride to obtain a low oxygen content characteristic The spherical aluminum nitride.
歸納前述,本發明鋁金屬直接製作球型氮化鋁之方法,其透過備料、造粒、篩選、混合及燒結等步驟,以直接利用純度80%以上的鋁金屬,並且該鋁金屬熱熔後,經一噴霧造粒機造粒形成一球型鋁粉,再利用篩選出小於一定粒徑以下範圍的球型鋁粉,使該球型鋁粉與促進劑以一定比例混合成一混合物後,再將該混合物置入高壓氣氛燒結爐,並以攝氏溫度為400以上,且壓力控制為50公斤以下,使該球型粉末進行轉化反應,形成一球型氮化鋁,如此將可快速、節能、低成本且可量產的製作出球型氮化鋁;此外,若適時將該球形氮化鋁接續有塗層步驟、高溫燒結步驟、精煉步驟,更可得到一低含氧量特性之球形氮化鋁。To summarize the foregoing, the method for directly producing spherical aluminum nitride from aluminum metal of the present invention uses the steps of material preparation, granulation, screening, mixing, and sintering to directly use aluminum metal with a purity of more than 80%, and the aluminum metal is hot melted , After being granulated by a spray granulator to form a spherical aluminum powder, the spherical aluminum powder smaller than a certain particle size is screened out, and the spherical aluminum powder and the accelerator are mixed into a mixture in a certain ratio, and then Put the mixture into a high-pressure atmosphere sintering furnace, and set the temperature above 400 degrees Celsius and control the pressure below 50 kg to make the spherical powder undergo a conversion reaction to form a spherical aluminum nitride, which will be fast, energy-saving, Low-cost and mass-produced spherical aluminum nitride; In addition, if the spherical aluminum nitride is followed by a coating step, a high-temperature sintering step, and a refining step, a spherical nitrogen with low oxygen content can be obtained. Aluminum.
惟以上所述者,僅為說明本發明之較佳實施例而已,當不能以此限定本發明實施之範圍,即大凡依本發明申請專利範圍及發明說明書內容所作之簡單的等效變化與修飾,皆應仍屬本發明專利涵蓋之範圍內。However, the above is only to illustrate the preferred embodiments of the present invention, and should not be used to limit the scope of implementation of the present invention, that is, simple equivalent changes and modifications made in accordance with the scope of the patent application of the present invention and the content of the description of the invention , Should still fall within the scope of the invention patent.
無no
圖1為習知製成所得之氮化鋁狀態圖。 圖2為本發明第一較佳實施例之流程方塊圖。 圖3為本發明製成所得之氮化鋁狀態圖。 圖4為本發明第二較佳實施例之流程方塊圖。Fig. 1 is a state diagram of the conventionally manufactured aluminum nitride. Fig. 2 is a block diagram of the first preferred embodiment of the present invention. Fig. 3 is a state diagram of aluminum nitride produced by the present invention. Fig. 4 is a block diagram of the second preferred embodiment of the present invention.
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