TWI707897B - 導熱性片 - Google Patents
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- TWI707897B TWI707897B TW109102498A TW109102498A TWI707897B TW I707897 B TWI707897 B TW I707897B TW 109102498 A TW109102498 A TW 109102498A TW 109102498 A TW109102498 A TW 109102498A TW I707897 B TWI707897 B TW I707897B
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- B29C48/0022—Combinations of extrusion moulding with other shaping operations combined with cutting
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Abstract
本發明係一種導熱性片之製造方法,其於製作導熱性片時無需使用高成本之磁性產生裝置,且可於熱硬化性樹脂組成物中大量地調配纖維狀填料,該導熱性片於配置於發熱體與散熱體之間時,即便不對該等施加如阻礙該等正常動作之負荷亦顯示出良好之導熱性,該導熱性片之製造方法具有如下步驟:步驟(A),其使纖維狀填料分散於黏合劑樹脂中,藉此製備導熱性片形成用組成物;步驟(B),其藉由擠出成形法或模具成形法從所製備之導熱性片形成用組成物形成出成形體塊;步驟(C),其將所形成之成形體塊切片成片狀;及步驟(D),其對所獲得之片之切片面進行加壓。
Description
本發明係關於一種導熱性片之製造方法。
為了防止驅動時伴隨著發熱之IC(integrated circuit)晶片等發熱體之故障,而使發熱體介隔導熱性片與散熱片等散熱體密合。近年來,提出有如下方法作為提高此種導熱性片之導熱性之方法:係使用磁場產生裝置,使於熱硬化性樹脂中分散有纖維狀填料之層狀熱硬化性樹脂組成物中之該纖維狀填料配向於層之厚度方向,之後使熱硬化性樹脂硬化而製造導熱性片(專利文獻1)。該導熱性片成為如下構成:纖維狀填料的端部露出於片之表面,當用於發熱體與散熱體之間時,纖維狀填料之露出之端部會沉入導熱性片內。
專利文獻1:日本專利第4814550號
[發明所欲解決之課題]
然而,於專利文獻1之技術中,存在如下問題:為了有意地使纖維狀填料配向,而必需使用高成本之磁性產生裝置。又,為了利用磁性產生裝置使纖維狀填料配向,而必需使熱硬化性樹脂組成物之黏度變低,因此存在如下問題:無法大幅增加纖維狀填料之含量,而導熱性片之導熱性變得不充分。進而,根據導熱性片應用於發熱體與散熱體之間之條件,亦存在露出之纖維狀填料之端部未沉入導熱性片內之問題。相反地為了使露出之纖維狀填料之端部完全地沉入導熱性片內,亦有存在如下情形之問題:將導熱性片配置於發熱體與散熱體之間時,不得不對該等施加如阻礙該等正常動作之負荷。
本發明之目的在於解決上述先前技術之問題點,從而可於製造導熱性片時無需使用高成本之磁性產生裝置,且可於熱硬化性樹脂組成物中大量地調配纖維狀填料,而製造於配置於發熱體與散熱體之間時,即便不對該等施加如阻礙該等正常動作之負荷亦顯示出良好之導熱性的導熱性片。
[解決課題之技術手段]
本發明人假設使纖維狀填料配向於導熱性片之厚度方向係引起先前技術之問題點之主要原因,於該假設下對纖維狀填料之配向狀態進行研究,結果發現,使黏合劑樹脂中相對多量地含有纖維狀填料而製備導熱性片形成用組成物,並且不使用磁性產生裝置來有意地使纖維狀填料配向,僅藉由擠出成形法或模具成形法從導熱性片形成用組成物形成出成形體塊,將其進行切片,進而進行加壓處理,藉此可製造可達成上述目的之導熱性片,從而完成本發明。
即,本發明提供一種導熱性片之製造方法,其係用於製造導熱性片者,且具有以下之步驟(A)~(D):
步驟(A)
使具有2~50之縱橫比的纖維狀填料分散於黏合劑樹脂中,藉此製備導熱性片形成用組成物之步驟;
步驟(B)
藉由擠出成形法或模具成形法從所製備之導熱性片形成用組成物形成出成形體塊之步驟;
步驟(C)
將所形成之成形體塊切片成片狀之步驟;及
步驟(D)
對所獲得之片之切片面進行加壓之步驟。
又,本發明提供一種藉由上述製造方法而獲得之導熱性片、以及將該導熱性片配置於發熱體與散熱體之間而成之感溫元件(thermal device)。
[發明之效果]
根據本發明之製造方法,使黏合劑樹脂中相對多量地含有纖維狀填料而製備導熱性片形成用組成物,並且僅藉由擠出成形法或模具成形法從導熱性片形成用組成物形成出成形體塊,將其進行切片,進而對所獲得之片進行加壓處理。因此,可認為雖一部分纖維狀填料沿成型時黏合劑樹脂之流動進行配向,但大部分纖維狀填料之配向變得無規則,藉由切片後之加壓來壓縮片,從而纖維狀填料於片內部相互接觸,因此可製造片內部之導熱性得到改善之導熱性片。並且可使片之表面平滑化,因此可製造與發熱體或散熱體之密合性變良好,當配置於發熱體與散熱體之間時即便不對該等施加如阻礙該等正常動作之負荷亦顯示出良好之導熱性之導熱性片。
本發明之導熱性片之製造方法具有以下之步驟(A)~(D)。對每個步驟詳細地進行說明。
<步驟(A)>
首先,使纖維狀填料分散於黏合劑樹脂中,藉此製備導熱性片形成用組成物。
構成導熱性片形成用組成物之纖維狀填料係用以使源自發熱體之熱效率良好地傳導至散熱體者。作為此種纖維狀填料,若平均徑過小,則擔心其比表面積變得過大,而導熱性片形成用組成物之黏度變得過高,若平均徑過大,則擔心導熱性片之表面凹凸變大,而對發熱體或散熱體之密合性下降,因此平均徑較佳為8~12 μm。又,若其縱橫比(長/徑)過小,則有導熱性片形成用組成物之黏度過高之傾向,若過大,則有阻礙導熱性片之壓縮之傾向,因此縱橫比較佳為2~50,更佳為3~30。
作為纖維狀填料之具體例,較佳為可列舉:碳纖維、金屬纖維(例如鎳、鐵等)、玻璃纖維、陶瓷纖維(例如氧化物(例如氧化鋁、二氧化矽等)、氮化物(例如氮化硼、氮化鋁等)、硼化物(例如硼化鋁等)、碳化物(例如碳化矽等)等非金屬系無機纖維)。
纖維狀填料係依導熱性片所要求之機械性質、熱性質、電性質等特性而選擇。其中,就顯示出高彈性率、良好之導熱性、高導電性、電波遮蔽性、低熱膨脹性等之方面而言,可較佳地使用瀝青(pitch)系碳纖維。
纖維狀填料於導熱性片形成用組成物中之含量有如下傾向:若過少則導熱率變低,若過多則黏度變高,因此纖維狀填料於導熱性片中之含量藉由調整各種材料之添加量較佳為16~40體積%,更佳為20~30體積%,且相對於構成導熱片形成用組成物之下述黏合劑樹脂100質量份,較佳為120~300質量份,更佳為130~250質量份。
再者,除纖維狀填料以外,亦可於無損本發明之硬化之範圍內併用板狀填料、鱗片狀填料、球狀填料等。特別是就抑制纖維狀填料於導熱性片形成用組成物中二次凝聚之觀點而言,0.1~5 μm直徑之球狀填料(較佳為球狀氧化鋁或球狀氮化鋁)之較佳範圍為30~60體積%,更佳為35~50體積%,且相對於纖維狀填料100質量份,較佳為併用100~900質量份。
黏合劑樹脂係將纖維狀填料保持於導熱性片內者,且依導熱性片所要求之機械強度、耐熱性、電性質等特性而選擇。作為此種黏合劑樹脂,可採用選自熱塑性樹脂、熱塑性彈性體、熱硬化性樹脂中者。
作為熱塑性樹脂,可列舉:聚乙烯、聚丙烯、乙烯-丙烯共聚物等乙烯-α烯烴共聚物、聚甲基戊烯、聚氯乙烯、聚偏二氯乙烯、聚乙酸乙烯酯、乙烯-乙酸乙烯酯共聚物、聚乙烯醇、聚乙烯醇縮醛、聚偏二氟乙烯及聚四氟乙烯等氟系聚合物、聚對苯二甲酸乙二酯、聚對苯二甲酸丁二酯、聚萘二甲酸乙二酯、聚苯乙烯、聚丙烯腈、苯乙烯-丙烯腈共聚物、丙烯腈-丁二烯-苯乙烯共聚物(ABS,acrylonitrile-butadiene-styrene)樹脂、聚苯醚共聚物(PPE,polyphenylene ether)樹脂、改質PPE樹脂、脂肪族聚醯胺類、芳香族聚醯胺類、聚醯亞胺、聚醯胺醯亞胺、聚甲基丙烯酸、聚甲基丙烯酸甲酯等聚甲基丙烯酸酯類、聚丙烯酸類、聚碳酸酯、聚伸苯硫、聚碸、聚醚碸、聚醚腈、聚醚酮、聚酮、液晶聚合物、聚矽氧樹脂、離子聚合物等。
作為熱塑性彈性體,可列舉:苯乙烯-丁二烯嵌段共聚物或其氫化物、苯乙烯-異戊二烯嵌段共聚物或其氫化物、苯乙烯系熱塑性彈性體、烯烴系熱塑性彈性體、氯乙烯系熱塑性彈性體、聚酯系熱塑性彈性體、聚胺基甲酸酯系熱塑性彈性體、聚醯胺系熱塑性彈性體等。
作為熱硬化性樹脂,可列舉:交聯橡膠、環氧樹脂、酚系樹脂、聚醯亞胺樹脂、不飽和聚酯樹脂、鄰苯二甲酸二烯丙酯(diallyl phthalate)樹脂等。作為交聯橡膠之具體例,可列舉:天然橡膠、丙烯酸系橡膠、丁二烯橡膠、異戊二烯橡膠、苯乙烯-丁二烯共聚合橡膠、腈橡膠、氫化腈橡膠、氯丁二烯橡膠、乙烯-丙烯共聚合橡膠、氯化聚乙烯橡膠、氯磺化聚乙烯橡膠、丁基橡膠、鹵化丁基橡膠、氟橡膠、胺基甲酸乙酯橡膠、及聚矽氧橡膠。
導熱性片形成用組成物可藉由利用公知之方法將纖維狀填料、黏合劑樹脂、及視需要而調配之各種添加劑或揮發性溶劑均勻地混合而製備。
<步驟(B)>
繼而,藉由擠出成形法或模具成形法從所製備之導熱性片形成用組成物形成出成形體塊。
作為擠出成形法、模具成形法,並無特別限制,可視導熱性片形成用組成物之黏度或導熱性片所要求之特性等,適當地從公知之各種擠出成形法、模具成形法中採用。
於擠出成形法中自模具擠出導熱性片形成用組成物時,或者於模具成形法中將導熱性片形成用組成物向模具壓入時,黏合劑樹脂會流動,一部分纖維狀填料會沿其流動方向進行配向,但大部分纖維狀填料之配向變得無規則。該情形時,若全纖維狀填料中配向變得無規則之纖維狀填料之比率(纖維狀填料之配向無規則率)過少,則有於下述步驟(D)之加壓後相互接觸之纖維狀填料之比率較少,而導熱性片之導熱性變得不足之傾向,若過多,則擔心片之厚度方向之導熱性變得不足,因此纖維狀填料之配向無規則率較佳為55~95%,更佳為60~90%。纖維狀填料之配向無規則率可藉由電子顯微鏡觀察進行計數。
再者,配向無規則率為0%之狀態意指單位立方體(例如0.5 mm見方)所含有之纖維狀填料全部配向於某固定方向(例如片厚度方向)的狀態。無規則率為100%之狀態意指單位立方體(例如0.5 mm見方)所含有之纖維狀填料中,配向於某固定方向(例如片厚度方向)之集合不存在的狀態。配向無規則率為50%之狀態意指單位立方體(例如0.5 mm見方)所含有之纖維狀填料中,屬於配向於某固定方向(例如片厚度方向)之集合之纖維狀填料之比率為50%的狀態。因此,配向無規則率為55%之狀態意指單位立方體(例如0.5 mm見方)所含有之纖維狀填料中,屬於配向於某固定方向(例如片厚度方向)之集合之纖維狀填料之比率為45%的狀態,配向無規則率為95%之狀態意指單位立方體(例如0.5 mm見方)所含有之纖維狀填料中,屬於配向於某固定方向(例如片厚度方向)之集合之纖維狀填料之比率為5%的狀態。
該配向無規則率可藉由如下方式算出:對片之一剖面進行觀察時,除去配置於厚度方向且可確認特定長度之纖維狀填料。又,可藉由增加觀察之剖面數,對所獲得之配向無規則率取平均數而提高其數值精度。
成形體塊之大小・形狀可依求出之導熱性片的大小而決定。例如可列舉剖面之縱向大小為0.5~15 cm且橫向大小為0.5~15 cm之長方體。長方體之長度視需要決定即可。
<步驟(C)>
繼而,將所形成之成形體塊切片成片狀。於藉由切片而獲得之片表面(切片面)纖維狀填料露出。作為切片之方法,並無特別限制,可根據成形體塊之大小或機械強度而自公知之切片裝置(較佳為超音波切割器)中進行適當選擇。作為成形體塊之切片方向,於成形方法為擠出成形法之情形時亦存在配向於擠出方向者,因此相對於擠出方向為60~120度、更佳為70~100度之方向。特佳為90度(垂直)之方向。
作為切片厚度,亦無特別限制,可根據導熱性片之使用目的等而適當選擇。
<步驟(D)>
繼而,對所獲得之片的切片面進行加壓。藉此可獲得導熱性片。作為加壓之方法,可使用由平盤與表面平坦之加壓頭所構成之一對加壓裝置。又,亦可利用夾送輥(pinch roll)進行加壓。
作為加壓時之壓力,通常若過低,則有未加壓之情形與熱阻未變化之傾向,若過高,則有片延伸之傾向。又,為了於加壓時防止延伸而使間隔物介存之情形時,可較高地設定加壓壓力。通常,對片施加之壓力為1~100 kgf/cm2
,但於未使用間隔物之情形時,較佳為2~8 kgf/cm2
,更佳為3~7 kgf/cm2
,於使用間隔物之情形時,加壓時之設定壓力為0.1~30 MPa,較佳為0.5~20 MPa。
於本發明中,作為間隔物,可使用與欲製作之片之厚度相同的由硬質材料所構成之框架或平板。例如,作為間隔物,可例示:於與欲製作之片之厚度相同之正方形(例如25 cm見方)的不鏽鋼板上設置4個正方形(例如10 cm見方)之洞,而製成如漢字“田”形狀之框架者,但並不限定於其。
為了更提高加壓效果,縮短加壓時間,上述加壓較佳為於黏合劑樹脂之玻璃轉移溫度以上時進行。通常於0~180℃之溫度範圍內,較佳為室溫(約25℃)~100℃之溫度範圍內,更佳為30~100℃之溫度範圍內進行加壓。
於本發明中,加壓後之片厚由於壓縮而變薄,但若片之壓縮率[{(加壓前之片厚-加壓後之片厚)/加壓前之片厚}×100]過小,則有熱阻不會變小之傾向,若過大,則有片延伸之傾向,因此以壓縮率成為2~15%之方式進行加壓。
又,可藉由加壓而使片之表面變平滑。平滑之程度能以表面光澤度(光澤值)進行評價。若表面光澤度過低,則導熱性下降,因此較佳為於入射角60度反射角60度下經光澤計所測定之表面光澤度(光澤值)成為0.2以上之方式進行加壓。
藉由以上說明之導熱性片之製造方法而獲得之該導熱性片亦為本發明之一態樣,其較佳態樣係纖維狀填料之配向無規則率為55~95%,厚度為0.1~50 mm,利用光澤計測出之表面光澤度(光澤值)成為0.2以上者。
此種導熱性片可供給一種感溫元件,其係為了將發熱體所產生之熱擴散至散熱體而配置於該等之間之結構。作為發熱體,可列舉IC(integrated circuit)晶片、IC模組等,作為散熱體,可列舉由不鏽鋼等金屬材料形成之熱槽(heat sink)等。
如以上所說明,導熱性片之熱特性較多係取決於所含有之纖維狀填料之配向無規則率,但該熱性質亦可以於片之厚度方向上纖維狀填料以何種角度之偏差排列而進行評價。具體而言,利用50~300倍之光學顯微鏡對導熱性片之一剖面進行拍攝,將片之表面方向設為90度時,採用攝影圖像而求出纖維狀填料之角度分佈,進而求出其標準偏差即可。標準偏差較佳為10°以上。
實施例
實施例1
將聚矽氧A液(具有乙烯基之有機聚矽氧烷)17體積%、聚矽氧B液(具有氫矽基(hydrogen silyl)之有機聚矽氧烷)16體積%、氧化鋁粒子(平均粒徑3 μm)22體積%、球狀之氮化鋁(平均粒徑1 μm)22體積%、及瀝青系碳纖維(平均長軸長150 μm、平均軸徑8 μm)23體積%均勻地進行混合,藉此製備導熱性片形成用聚矽氧樹脂組成物。若以質量份進行換算,則相對於聚矽氧樹脂100質量份,將瀝青系碳纖維153質量份進行混合而製備導熱性片形成用聚矽氧樹脂組成物。
將該導熱性片形成用聚矽氧樹脂組成物灌入長方體狀之具有內部空間之模具中,於100℃之烘箱中加熱硬化6小時,藉此製作成形體塊。再者,於模具之內面以剝離處理面成為內側之方式貼附剝離聚對苯二甲酸乙二酯膜。
利用超音波切割器將所獲得之成形體塊切片成0.2 mm厚而獲得片。於該片之表面,由於切片時之剪力故纖維狀填料之一部分會露出於表面,而於片表面形成有微小之凹凸。
將以上述方式獲得之片載置於不鏽鋼壓盤上,以對片施加2 kgf/cm2
之荷重之方式,於常溫(25℃)下利用表面經鏡面精加工之平坦的不鏽鋼加壓頭進行30分鐘加壓,藉此獲得表面平滑之導熱性片。將該加壓後之片厚與壓縮率示於表1。
再者,利用100倍之光學顯微鏡對導熱性片之平面進行拍攝,將片之表面方向設為90度時,採用攝影圖像而求出纖維狀填料之角度分佈,進而求出其標準偏差。角度分佈之平均為-12.9°且標準偏差為15.6°。
實施例2~45、比較例1
如表1所示變更實施例之成形體塊之切片厚度、加壓條件(壓力、溫度),除此以外,以與實施例1相同之操作獲得導熱性片。又,將加壓後之片厚與壓縮率示於表1。
比較例1
除不進行加壓以外,以與實施例1相同之操作獲得導熱性片。
實施例46~51
如表1所示,變更實施例之成形體塊之切片厚度、加壓條件(壓力、溫度)、瀝青系碳纖維之平均長軸長(μm)與平均軸徑(μm),又,於加壓時使用間隔物(於具有與欲製作之片之厚度相同厚度之25 cm見方的不鏽鋼板上設有4個10 cm見方之洞者),進而,關於實施例46、47,於聚矽氧樹脂100質量份中混合碳纖維240質量份,關於實施例48~51,於聚矽氧樹脂100質量份中混合碳纖維150質量份,除此以外,以與實施例1相同之操作獲得導熱性片。將加壓前後之片厚與壓縮率示於表1。
<評價>
針對所獲得之導熱性片,將對片施加之壓力設為表1所示之數值,並且使用依據ASTM-D5470之熱阻測定裝置而對各自之熱阻[(K/W)以及(K・cm2
/W)]進行測定。將所獲得之結果示於表1。期望於實際使用時,熱阻於加壓前之片厚為0.1 mm以上且未達0.2 mm時為0.4 K/W(1.256(K・cm2
/W))以下,於片厚為0.2 mm以上且未達0.6 mm時為0.130 K/W(0.41(K・cm2
/W))以下,於片厚為0.6 mm以上且未達1.0 mm時為0.140 K/W(0.44(K・cm2
/W))以下,於片厚為1.0 mm以上且未達3.0 mm時為0.5 K/W(1.57(K・cm2
/W))以下。
又,關於實施例6、10、21、25、46~51及比較例1,使用光澤度計(入射角60度、反射角60度)測定表面光澤度(光澤值)。將所獲得之結果示於表1。
表1之實施例1~45之導熱性片於加壓後各片厚中分別顯示出良好之較低熱阻。又,測定出表面光澤度之實施例6、10、21、25之導熱性片之表面光澤度(光澤值)為0.2以上。
又,可知存在如下傾向,即隨著加壓壓力上升而熱阻下降、隨著加壓溫度上升而熱阻上升、及隨著片厚變厚而熱阻上升。
另一方面,於未實施加壓之比較例1之導熱性片之情形時,熱阻超過0.130 K/W,並且光澤值為0.1,表面光澤度較低。
又,於實施例46之導熱性片之情形時,於加壓時使用間隔物,因此將加壓溫度設定為較高之100℃,並且碳纖維之平均長軸長相對較短為100 μm,因此片之壓縮率為67%,非常高。因此,於加壓前為0.10 mm之片厚,顯示出良好之較低熱阻。又,表面光澤度(光澤值)為0.1以上。
於實施例47之導熱性片之情形時,將加壓溫度設定為70℃,除此以外,重複與實施例46相同之操作。因此,與實施例46之情形相比,壓縮率變低為約43%,但於加壓前為0.10 mm之片厚,顯示出良好之較低熱阻。又,表面光澤度(光澤值)為0.1以上。
於實施例48~51之導熱性片之情形時,於加壓時使用間隔物,並且片厚相對較厚,但將加壓壓力設定為相對較高之1.2~20 MPa,因此於加壓前為1.55~2.54 mm之片厚,顯示出良好之較低熱阻。又,表面光澤度(光澤值)為0.2以上。
[產業上之可利用性]
根據本發明之製造方法,可製造一種大部分纖維狀填料於成形時配向變得無規則,但藉由切片後之加壓而壓縮片,從而纖維狀填料於片內部相互接觸,因此片內部之導熱性得到改善之導熱性片。並且因可使片之表面平滑化,故可製造一種與發熱體或散熱體之密合性變良好,於配置於發熱體與散熱體之間時,即便不對該等施加如阻礙該等正常動作之負荷亦顯示出良好導熱性之導熱性片。因此,本發明可用於製造用以配置於IC晶片或IC模組等發熱體與散熱體之間之導熱性片。
無。
無。
Claims (4)
- 一種導熱性片,其含有導熱性片形成用組成物,上述導熱性片形成用組成物係藉由將由碳纖維或金屬纖維構成之纖維狀填料及球狀填料分散於黏合劑樹脂中而獲得,上述纖維狀填料具有2~50之縱橫比,且,伴隨著上述黏合劑樹脂之流動或變形,上述纖維狀填料於片內部相互接觸,配向變得無規則;上述導熱性片形成用組成物形成為片狀時,其片之表面光澤度(光澤值)為0.1以上;上述導熱性片形成用組成物中之纖維狀填料及球狀填料之添加量分別為16~40體積%及30~60體積%;上述導熱性片中,纖維狀填料之配向無規則率為55~95%。
- 如申請專利範圍第1項之導熱性片,其中,上述導熱性片形成用組成物形成為片狀時,其片之表面光澤度(光澤值)為0.2以上。
- 如申請專利範圍第1或2項之導熱性片,其中,上述導熱性片形成用組成物中之纖維狀填料及球狀填料之添加量分別為20~30體積%及35~50體積%。
- 如申請專利範圍第1或2項之導熱性片,其中,纖維狀填料之配向無規則率為60~90%。
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TW104106473A TWI589626B (zh) | 2012-07-07 | 2013-07-05 | Method of manufacturing a thermally conductive sheet |
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