TWI474991B - 製備球型氮化硼聚集體之漿料及其應用 - Google Patents
製備球型氮化硼聚集體之漿料及其應用 Download PDFInfo
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Description
本發明係關於一種用於製備球型氮化硼聚集體之漿料,特別係關於一種可在相對低之溫度下製備球型氮化硼聚集體之漿料。
六方氮化硼,為高溫工業、化妝品工業、高分子工業、電子工業與光電產業上游產品,是各種高溫保護、高溫潤滑、導熱散熱等的關鍵填充材料,可用於製造高溫離型劑、高溫潤滑劑、化妝品添加劑、導熱散熱添加劑及薄膜導熱介面材料。
傳統六方氮化硼(BN)為扁平形貌,雖具許多絕佳特性,例如:高熱傳導係數,高絕緣特性,疏水性,化學穩定性及潤滑性等,但粉體易凝聚成團。做為填充劑(filler)時,一般氮化硼添加劑在其添加量超過30%時,將造成漿料黏度增加而難以做後續製程,且添加量也難以進一步增加。故對於其產品功能也難以大幅提昇。另一方面直接以粉體狀態與溶劑摻混,不但操作性差(例如黏度過高),同時凝團使得複合材料的許多性能受到壓制。傳統技術上為了克服此一缺點,材料供應商先將粉體與溶劑混合並進行研磨,待粒徑達到要求後(例如<1μm),再將溶劑揮發,獲得乾式粉體,再交由使用者與高分子摻混。然而此種方法,不但耗費工時,又增加成本。並且,且相對於一般易分散的填充材料的使用,如氧化鋁(Al2
O3
)或氧化鋅(ZnO)等,BN仍然有使用不方便,分散不易等缺點,使得六方氮化硼的應用受到限制。
另一方面為改進此項缺點,將氮化硼球型化是目前許多單位努力的目標。傳統之方法係利用添加有機金屬醋酸鹽(metal acetate)作為黏結劑,製成球型氮化硼聚集體。然,於此方法中,有機金屬醋酸鹽將變成BN粉體的一部份而影響氮化硼之功能。為進一步將有機金屬醋酸鹽形成較為無害的無機氧化物陶瓷,需再進行1500℃持溫一小時以上的熱處理。如此一來,相當耗能,所需成本亦相對較高。再者,氮化硼在過高之溫度下易於氧化,因此,習知之方法需於特定之環境氛圍下保護氮化硼進行熱處理,大幅提升製程的困難度。
上述缺失均降低氮化硼之後續應用性,因此,如何開發出一種改善習知氮化硼球型化製程之缺失,以提升氮化硼之應用性,實為一個重要之課題。
有鑒於此,本發明之目的係開發出一種用於製備球型氮化硼聚集體之漿料,其係可在相對低的溫度下製備出球型氮化硼聚集體,進而達到省能及製造成本之訴求。
此外,本發明之另一目的係開發一種在低溫下製造球型氮化硼聚集體之方法,其主要係透過添加固態黏結劑來降低製程中燒結所需之溫度。
為達上述目的,本發明係提供一種用於製備球型氮化硼聚集體之漿料,其包含:3重量%~25重量%之氮化硼;1重量%~25重量%之奈米陶瓷材料;及一溶劑,其作為補足至100重量%之補充物。
於一較佳實施態樣中,該奈米陶瓷材料係金屬氧化物、非金屬碳化物或金屬奈米粒子。該氧化物較佳係氧化鋅、二氧化鈦、或氧化鋁;該非金屬碳化物較佳係碳化矽。
於一較佳實施態樣中,該溶劑係水或醇類。
本發明另提供一種製備球型氮化硼聚集體之方法,其包含:(a)提供一氮化硼及一奈米陶瓷材料;(b)將該氮化硼及該奈米陶瓷材料分散於一溶劑中,得一漿料;(c)調整該漿料之pH值;及(d)噴霧乾燥並燒結,得一球型氮化硼聚集體。
於一較佳實施態樣中,該奈米陶瓷材料係金屬氧化物、非金屬碳化物或金屬奈米粒子。該氧化物較佳係氧化鋅、二氧化鈦、或氧化鋁;該非金屬碳化物較佳係碳化矽。
於一較佳實施態樣中,該pH值係介於4~8之間。
於一較佳實施態樣中,該方法係於該步驟(c)後進一步包含一球磨之步驟。
於一較佳實施態樣中,該方法係於該球磨步驟後進一步包含加入一界面活性劑之步驟。該界面活性劑較佳係聚乙烯醇或聚丙烯酸銨(Ammonium polyacrylate)。
於一較佳實施態樣中,該燒結步驟係於350℃~1000℃間進行。更佳係於500℃~900℃間。
本發明主要係利用奈米陶瓷材料燒結溫度低之特性,來降低球型化製程中熱處理所需之溫度,進而達到省能及低成本之訴求。並且,由於本發明之方法僅需於不高於1000℃之溫度下進行熱處理,因此,無需於特定之環境氛圍下保護氮化硼,進而可降低製程之困難度。
本發明係提供一種可在相對低之溫度下製備出球型氮化硼聚集體之漿料,其可在不高於1000℃之溫度下製備出球型氮化硼聚集體。
具體而言,本發明所提供之用於製備球型氮化硼聚集體之漿料,其包含:3重量%~25重量%之氮化硼;1重量%~25重量%之奈米陶瓷材料;及一溶劑,其作為補足至100重量%之補充物。
而本發明所提供之製備球型氮化硼聚集體之方法,其包含:(a)提供一氮化硼及一奈米陶瓷材料;(b)將該氮化硼及該奈米陶瓷材料分散於一溶劑中,得一漿料;(c)調整該漿料之pH值;及(d)噴霧乾燥並燒結,得一球型氮化硼聚集體。
於本發明中,該奈米陶瓷材料係扮演固體黏結劑之角色,其包含但並不限於:金屬氧化物(諸如:氧化鋅、二氧化鈦、或氧化鋁)、非金屬碳化物(諸如:碳化矽)或金屬奈米粒子(諸如:鎳、鈦、鋁、銅或其合金)。於實際使用時,使用者可依其功能性選擇不同之奈米陶瓷材料,舉例來說,氮化硼作為化妝品添加劑使用時,可選用二氧化鈦作為奈米陶瓷材料,使球型化之氮化硼除了具有原先特性外,兼具抗紫外線照射之功能。
當可輕易理解的是,本發明所用之溶劑並無特別之限定,只要其可使氮化硼及奈米陶瓷材料分散於其中即可。該溶劑包含水或醇類,但並不限於此。
於本發明之方法中係使用鹼液或酸液調整該漿料之pH值,該鹼液較佳係NaOH或NH3
水溶液;該酸液較佳係HCl水溶液。而該漿料之pH值較佳係調整至4~8之間。此外,為了使調整pH值後所得之漿料中氮化硼及奈米陶瓷材料更均勻地分散於溶劑中,係可對該調整後之漿料進行球磨來打散溶劑中的團聚粉體。進一步地,係可將一界面活性劑添加入球磨後所得之漿料中,再進行後續噴霧乾燥及燒結之步驟。該界面活性劑包含聚乙烯醇(polyvinyl alcohol)或聚丙烯酸銨(Ammonium polyacrylate),但並不限於此。
本發明中所稱之「噴霧乾燥」及「燒結」均為本領域技術人員所熟知之技術,因此,本文中不再贅述。而值得注意的是,本發明藉由添加作為固體黏結劑之奈米陶瓷材料,可將燒結之溫度降低至350℃~1000℃間進行,進而可降低製造成本及製造之困難度。
本發明之技術特徵已具體敘述於發明說明中,其他各項之材料與配方係屬於習知技藝,本領域熟知該項技藝者當可輕易實施本發明。以下將藉由實施例的方式例示本發明之特徵與優點。
以40克之六方氮化硼及60克之奈米級二氧化鈦(TiO2
)作為起始原料,其中該六方氮化硼之平均粒徑4μm,而二氧化鈦的粒徑分佈為30~50nm。將氮化硼與TiO2
分散入400mL之去離子水中均勻攪拌,得一漿料。接著以鹽酸及NaOH水溶液調整pH值,使之pH值為4。接著,將調整後之漿料進行球磨,再加入10克之2重量%的聚乙烯醇(PVA)水溶液。所得之溶液再以噴霧乾燥器(CNK-SDD-0100)進行噴霧乾燥,得氮化硼-二氧化鈦複合粉體,該噴霧乾燥之條件係進口溫度為200℃,出口溫度為120℃,轉速為3000rpm,進料速度為1.5公升/小時。將該氮化硼-二氧化鈦複合粉體於800℃進行燒結,即得本發明之球型氮化硼聚集體-1(90g)。
第一圖A係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結前之巨觀SEM圖(100X)。第一圖B係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結後之巨觀SEM圖(600X)(即本發明之球型氮化硼聚集體-1之巨觀SEM圖)。由第一圖B之結果顯示,本發明之球型氮化硼聚集體-1之粒徑約為20~50μm。
第二圖A係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結前之微觀SEM圖(2000X)。第二圖B係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結後之微觀SEM圖(1900X)(即本發明之球型氮化硼聚集體-1之微觀SEM圖)。由第二圖A之結果顯示,燒結前粉體之表面係有一層薄膜存在,該薄膜即為界面活性劑。而由第二圖B之結果顯示,粉體燒結後,原先之薄膜已消失不存在,證實該絕大部分之界面活性劑確已被移除。因此,本發明之球型氮化硼聚集體不會因大量界面活性劑之殘留而影響其功能。
除了將起始原料改成45克之六方氮化硼及45克之奈米級氧化鋁(Al2
O3
)外,其餘條件與實施例1相同,以製得氮化硼-氧化鋁複合粉體。接著將該氮化硼-氧化鋁複合粉體於800℃進行燒結,即得本發明之球型氮化硼聚集體-2(81g)。
第三圖A係顯示實施例2之氮化硼-氧化鋁複合粉體燒結前之巨觀SEM圖(300X)。第三圖B係顯示實施例2之氮化硼-氧化鋁複合粉體燒結後之巨觀SEM圖(1000X)。由第三圖之結果顯示,本發明之球型氮化硼聚集體-2之粒徑約為20-80μm,且其形狀況良好。
第四圖A係顯示實施例2之氮化硼-氧化鋁複合粉體燒結前之微觀SEM圖(20000X)。第四圖B係顯示實施例2之氮化硼-氧化鋁複合粉體燒結後之微觀SEM圖(50000X)(即為第四圖A圈選處之放大SEM圖),其中顆粒狀之部分為Al2
O3
,片狀部分即為氮化硼。結果顯示,燒結後,絕大部分之界面活性劑已被移除,而且氧化鋁有彼此燒結的現象。
除了將起始原料改成72克之六方氮化硼及18克之奈米級氧化鋁(Al2
O3
)外,其餘條件與實施例1相同,以製得氮化硼-氧化鋁複合粉體。接著將該氮化硼-氧化鋁複合粉體於800℃進行燒結,即得本發明之球型氮化硼聚集體-3(81g)。
第五圖A係顯示實施例3之球型氮化硼聚集體之巨觀SEM圖(300X)。第五圖B係顯示實施例3之球型氮化硼聚集體之微觀SEM圖(3000X)。第五圖C係顯示實施例3之球型氮化硼聚集體表面之SEM圖(50000X)。由第五圖A及第五圖B之結果顯示,本發明之球型氮化硼聚集體-3之粒徑約為20~80μm,並且成形良好。而由第五圖C之SEM圖可發現,本發明之球型氮化硼聚集體-3之表面幾乎皆為氮化硼,而未發現氧化鋁。
綜上所述,相較於習知製備球型氮化硼聚集體之方法,本發明所提供之方法係可在較低的溫度下進行熱處理,進而可降低能耗、製備成本及製作困難度。所得之球型氮化硼聚集體則因表面界面活性劑殘留量少,因此,其功能不受影響,進而大幅提升氮化硼之應用性。
所有揭露於本發明書之特徵係可使用任何方式結合。本說明書所揭露之特徵可使用相同、相等或相似目的的特徵取代。因此,除了特別陳述強調處之外,本說明書所揭露之特徵係為一系列相等或相似特徵中的一個實施例。
此外,依據本說明書揭露之內容,熟悉本技術領域者係可輕易依據本發明之基本特徵,在不脫離本發明之精神與範圍內,針對不同使用方法與情況作適當改變與修飾,因此,其它實施態樣亦包含於申請專利範圍中。
第一圖A係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結前之巨觀SEM圖(100X)。
第一圖B係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結後(即本發明之球型氮化硼聚集體)之巨觀SEM圖(600X)。
第二圖A係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結前之微觀SEM圖(2000X)。
第二圖B係顯示實施例1之氮化硼-二氧化鈦複合粉體燒結後(即本發明之球型氮化硼聚集體)之微觀SEM圖(1900X)。
第三圖A係顯示實施例2之氮化硼-氧化鋁複合粉體燒結前之巨觀SEM圖(300X)。
第三圖B係顯示實施例2之氮化硼-氧化鋁複合粉體燒結後(即本發明之球型氮化硼聚集體)之巨觀SEM圖(1000X)。
第四圖A係顯示實施例2之氮化硼-氧化鋁複合粉體燒結前之微觀SEM圖(20000X)。
第四圖B係顯示實施例2之氮化硼-氧化鋁複合粉體燒結後(即本發明之球型氮化硼聚集體)之微觀SEM圖(50000X)。
第五圖A係顯示實施例3之球型氮化硼聚集體之巨觀SEM圖(300X)。
第五圖B係顯示實施例3之球型氮化硼聚集體之微觀SEM圖(3000X)。
第五圖C係顯示實施例3之球型氮化硼聚集體表面之SEM圖(50000X)。
Claims (9)
- 一種用於製備球型氮化硼聚集體之漿料,其包含:3重量%~25重量%之氮化硼;1重量%~25重量%之奈米陶瓷材料;及一溶劑,其作為補足至100重量%之補充物,其中,該奈米陶瓷材料係非金屬碳化物。
- 如申請專利範圍第1項所述之漿料,其中該非金屬碳化物係碳化矽。
- 如申請專利範圍第1項所述之漿料,其中該溶劑係水或醇類。
- 一種製備球型氮化硼聚集體之方法,其包含:(a)提供一氮化硼及一奈米陶瓷材料;(b)將該氮化硼及該奈米陶瓷材料分散於一溶劑中,得一漿料;(c)調整該漿料之pH值;及(d)噴霧乾燥並於350℃~1000℃間進行燒結,得一球型氮化硼聚集體,其中,該奈米陶瓷材料係非金屬碳化物。
- 如申請專利範圍第4項所述之方法,其中該非金屬碳化物係碳化矽。
- 如申請專利範圍第4項所述之方法,其中該pH值係介於4~8之間。
- 如申請專利範圍第4項所述之方法,其係於該步驟(c)後進一步包含一球磨之步驟。
- 如申請專利範圍第7項所述之方法,其係於該球磨步驟後進一步包含加入一界面活性劑之步驟。
- 如申請專利範圍第8項所述之方法,其中該界面活性劑係聚乙烯醇或聚丙烯酸銨(Ammonium polyacrylate)。
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EP3464175A4 (en) | 2016-05-27 | 2019-12-11 | Saint-Gobain Ceramics & Plastics Inc. | METHOD FOR MANUFACTURING BORON NITRIDE AGGLOMERATES |
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