TWI825384B - 緻密質複合材料、其製法、接合體及半導體製造裝置用構件 - Google Patents

緻密質複合材料、其製法、接合體及半導體製造裝置用構件 Download PDF

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TWI825384B
TWI825384B TW110102032A TW110102032A TWI825384B TW I825384 B TWI825384 B TW I825384B TW 110102032 A TW110102032 A TW 110102032A TW 110102032 A TW110102032 A TW 110102032A TW I825384 B TWI825384 B TW I825384B
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composite material
dense composite
less
silicon carbide
titanium
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TW110102032A
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TW202142520A (zh
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永井明日美
西村昇
山口浩文
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日商日本碍子股份有限公司
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Abstract

本發明之緻密質複合材料含有矽化鈦43~63質量%，並且含有碳化矽及碳化鈦各少於矽化鈦之質量%，碳化矽之粒子間距離的最大值係40μm以下，標準偏差係10以下，開孔孔隙度係1%以下。

Description

緻密質複合材料、其製法、接合體及半導體製造裝置用構件
本發明係有關於緻密質複合材料、其製法、接合體及半導體製造裝置用構件。
在半導體製程中會高溫化之靜電吸盤接合有冷卻板以進行散熱。此時，有使用氧化鋁作為靜電吸盤之材料，使用鋁作為冷卻板之材料，使用樹脂作為接合材之情形。氧化鋁與鋁之線膨脹係數差非常大，舉例而言，氧化鋁之線膨脹係數為7.9ppm/K(RT-800℃：內田老鶴圃「陶瓷之物理」)，鋁之線膨脹係數為31.1ppm/K(RT-800℃：日本熱物理性質學會編、「新編熱物理性質手冊」)。將靜電吸盤與冷卻板接合時，冷卻板所需之特性例如有與靜電吸盤之線膨脹係數差小、為維持散熱性而熱傳導率高、為使冷卻液或冷卻氣體通過而緻密性高、為經得起加工或安放等而強度高等。滿足此種特性之材料例如有揭示於專利文獻1之複合材料。此複合材料含有碳化矽粒子37~60質量%，並且含有矽化鈦、碳化鈦矽及碳化鈦各少於碳化矽粒子之質量%，開孔孔隙度為1%以下。此複合材料之與氧化鋁的線膨脹係數差極小，熱傳導率、緻密性及強度足夠高。 [先前技術文獻] [專利文獻]
[專利文獻1]日本專利公報第6182082號
[發明欲解決之問題]
然而，專利文獻1之複合材料有隨著批別的不同而產生燒結不良部之情形。其理由如下。專利文獻1之複合材料的矽化鈦相、碳化鈦矽相及碳化鈦相的分布反映了燒成前之成形體中的金屬鈦粒子之配置。因此，當存在許多粒徑大之金屬鈦粒子時，金屬鈦粒子之配置會變得不均勻，而產生含鈦相與碳化矽粒子之偏析部。結果，鈦成分無法充分進入碳化粒子彼此之間隙，而產生燒結不良部(空隙)。
本發明係為了解決上述問題進行研發而成，其主要目的係提供具有與氧化鋁之線膨脹係數差極小，熱傳導率、緻密性及強度足夠高之特性的燒結性高之材料。 [解決問題之手段]
本發明之緻密質複合材料含有二矽化鈦43~63質量%，並且含有碳化矽及碳化鈦各少於二矽化鈦之質量%，碳化矽之粒子間距離的最大值係40μm以下，標準偏差係10以下，開孔孔隙度係1%以下。
此外，在本說明書中顯示數值範圍之「~」係當作包含記載於其前後之數值作為下限值及上限值之意來使用。
本發明之接合體係接合了由此種緻密質複合材料構成的第1材與由氧化鋁構成之第2材，本發明之半導體製造裝置用構件係利用此種接合體之構件。
本發明的緻密質複合材料之製法包含有下列製程：(a)調製一種粉體混合物，該粉體混合物含有平均粒徑為10~25μm之碳化矽24~45質量%、平均粒徑不足10μm之矽化鈦42~67質量%，並且含有平均粒徑不足20μm之金屬鈦或平均粒徑不足10μm之碳化鈦；(b)在惰性氣體環境下以熱壓使該粉體混合物以1350~1430℃燒結。 [發明之效果]
本發明之緻密質複合材料係具有與氧化鋁之線膨脹係數差極小，熱傳導率、緻密性及強度足夠高之特性的燒結性高之材料。因此，由於接合了由此種緻密質複合材料構成之第1材與由氧化鋁構成之第2材的接合體可利用作為半導體製造裝置用構件，即使在低溫與高溫之間重複使用，第1材與第2材亦不致剝落，故就在維持著高散熱性能之狀態下，耐用期間長久。又，本發明的緻密質複合材料之製法適合製造上述緻密質複合材料。
[發明之實施形態]
本實施形態之緻密質複合材料含有矽化鈦43~63質量%，並且含有碳化矽及碳化鈦各少於矽化鈦之質量%，碳化矽之粒子間距離的最大值係40μm以下，標準偏差係10以下，開孔孔隙度係1%以下。
本實施形態之緻密質複合材料含有矽化鈦43~63質量%。含有量係以裏特沃爾德分析所得之值。當矽化鈦含有量未達43質量%時，由於隨著製造批別的不同有時會產生燒結不良部之情形，故不符合期待。又，當含有矽化鈦超過63質量%時，由於緻密質複合材料之熱膨脹係數過大，與氧化鋁之熱膨脹係數差增大，而有接合體之第1材與第2材剝落的可能性，故不符合期待。矽化鈦可舉TiSi2 、TiSi、Ti5 Si4 、Ti5 Si3 等為例，當中以TiSi2 為佳。
本實施形態之緻密質複合材料含有碳化矽(SiC)及碳化鈦(TiC)各少於矽化鈦之質量%。碳化矽之質量%以大於碳化鈦之質量%為佳。以含有碳化矽29~46質量%為佳。碳化矽之平均粒子徑以10~25μm為佳。以含有碳化鈦5~15質量%為佳。
本實施形態之緻密質複合材料的碳化矽之粒子間距離的最大值為40μm以下且碳化矽之粒子間距離的標準偏差為10以下。當不滿足此條件時，有時會無法獲得足夠高之強度或燒結性不足，故不符合期待。碳化矽之粒子間距離的平均值以4~10μm為佳。碳化矽之粒子間距離可藉分析緻密質複合材料之SEM圖像而求出。
本實施形態之緻密質複合材料的開孔孔隙度為1%以下。開孔孔隙度係以將純水作為介質之阿基米德法測定的值。開孔孔隙度以0.1%以下為佳。
本實施形態之緻密質複合材料的線膨脹係數與氧化鋁相同程度。因此，將以本實施形態之緻密質複合材料製作的構件與以氧化鋁製作的構件接合(例如金屬接合)時，即使在低溫與高溫之間重複使用，亦不易剝落。具體而言，本實施形態之緻密質複合材料的與氧化鋁之40~570℃之平均線膨脹係數的差之絕對值以0.5ppm/K以下為佳，以0.3ppm/K以下為較佳。又，本實施形態之緻密質複合材料的40~570℃之平均線膨脹係數以7.2~8.2ppm/K為佳，以7.4~8.0ppm/K為較佳。
本實施形態之緻密質複合材料的熱傳導性優異，具體而言，熱傳導率以70W/mK以上為佳。如此一來，當將以本實施形態之緻密質複合材料製作的構件與以氧化鋁製作的構件進行金屬接合時，可以高效率地釋放氧化鋁具有之熱。
本實施形態之緻密質複合材料的強度優異，具體而言，四點抗彎強度以250MPa以上為佳。如此一來，易將以本實施形態之緻密質複合材料製作的構件應用於冷卻板等。
本實施形態之緻密質複合材料亦可含有碳化鈦矽。當含有碳化鈦矽時，其含有率以10質量%以下為佳，以0.5~9質量%為較佳。碳化鈦矽以Ti3 SiC2 (TSC)為佳。
本實施形態之接合體係接合(例如金屬接合)了以上述緻密質複合材料製作的第1材與以氧化鋁製作之第2材的接合體。此種接合體可應用於例如半導體製造裝置用構件。半導體製造裝置用構件可舉例如以將鋁或其合金作為主成分之接合材接合以上述緻密質複合材料製作之冷卻板(第1材)與以氧化鋁製作之靜電吸盤(第2材)之構件等為例。第1材由於與氧化鋁之線膨脹係數差極小，故即使在低溫與高溫重複使用，亦不易從第2材剝落。又，第1材由於熱傳導率足夠高，故可以高效率地冷卻以氧化鋁製作之第2材。再者，第1材由於緻密性足夠高，故可使冷卻液或冷卻氣體通過內部，冷卻效率進一步提高。又，第1材由於強度足夠高，故亦可十分經得起製造前述半導體製造裝置用構件之際的加工或接合、因使用作為構件之際的溫度差而產生之應力。
本實施形態的緻密質複合材料之製法包含有下列製程：(a)調製一種粉體混合物，該粉體混合物含有平均粒徑為10~25μm之碳化矽24~45質量%、平均粒徑不足10μm之矽化鈦42~67質量%，並且含有平均粒徑不足20μm之金屬鈦或平均粒徑不足10μm之碳化鈦；(b)在惰性氣體環境下以熱壓使該粉體混合物以1350~1430℃燒結。
由於在製程(a)，調製粉體混合物時，將各成分(碳化矽、矽化鈦、金屬鈦及碳化鈦)之平均粒徑設定成落入上述數值範圍，將各成分之含有率設定成落入上述數值範圍，故在製程(b)使該粉體混合物燒結後而得之緻密質複合材料易形成為具有與氧化鋁之線膨脹係數差極小，熱傳導率、緻密性及強度足夠高之特性的燒結性高之材料。此製法適合製造本實施形態之緻密質複合材料。
在製程(a)，關於粉體混合物中之源自碳化矽以外的原料之Si及Ti，Si/(Si+Ti)之質量比係0.40~0.50。
在製程(b)，惰性氣體環境可舉真空氣體環境、氬氣氣體環境、氦氣體環境或氮氣體環境等為例。熱壓燒成時之加壓壓力並未特別限定，以在50~300kgf/cm2 設定為佳。此外，燒成時間按燒成條件，適宜設定即可，例如在1~10小時之間適宜設定即可。
此外，本發明絲毫不受限於上述實施形態，只要屬於本發明之技術範圍，可以各種態樣實施是無須贅言的。 [實施例]
以下，就本發明之較佳的應用例作說明。SiC原料使用了純度97%以上、平均粒徑15.5μm之市售品。金屬Ti原料使用了純度99.5%以上、平均粒徑12.9μm之粉末。二矽化鈦使用了純度99%以上、平均粒徑6.9μm之市售品。碳化鈦使用了純度99%以上、平均粒徑4.3μm之市售品。此外，以下之實施例絲毫未限定本發明。
[實驗例1~11] 1.製造程序 •調和 將各原料成分秤量成表1所示之質量%，以異丙醇為溶媒，使用尼龍製鍋、直徑10mm之含鐵芯尼龍球，進行濕式混合4小時。取出混合後漿料，在氮氣流中以110℃乾燥。之後，通過30目篩網，形成為調和粉末。此外，確認了將所秤量之原料約500g投入至高速流動混合機(粉體投入部之容量1.8L)，以攪拌葉片之轉速1500rpm混合時，亦獲得了與濕式混合相同之材料特性。 •成形 以200kgf/cm2 之壓力將調和粉末單軸加壓成形，製作直徑50mm、厚度17mm左右之圓盤狀成形體，收納於燒成用石墨模具。 •燒成 藉將圓盤狀成形體熱壓燒成，而獲得了緻密質燒結材料。在熱壓燒成，令加壓壓力為200kgf/cm2 ，以表1所示之燒成溫度(最高溫度)燒成，在燒成結束前為真空氣體環境。燒成溫度之保持時間為4小時。
2.表之說明 於表1顯示了a：各實驗例之起始原料組成(調和比)、b：原料中源自SiC以外之成分(Si、Ti、TiSi2 、TiC)的Si對Si、Ti之總量的質量比(Si/(Si+Ti))、c：燒成條件(熱壓燒成溫度及加壓載重)、d：從裏特沃爾德分析求出之複合材料的組成相與其質量比、e：複合材料之基本特性(有關於體積密度、開孔孔隙度、四點抗彎強度、線膨脹係數、熱傳導率、碳化矽之粒子間距離的參數)。此外，實驗例1~11中，實驗例1~9相當於本發明之實施例，其餘之實驗例則相當於比較例。
[表1]
實驗例 1 2 3 4 5 6 7 8 9 10 11
a.原料調和比    mass% SiC 42.7 44.7 34.7 34.7 34.7 34.7 34.6 24.7 24.7 42.7 42.7
Si - - - - - - - - - 22.7 22.7
Ti 14.8 - - - - - - - - 34.6 34.6
TiSi2 42.5 48.9 47.7 52.7 52.7 52.7 58.5 54.9 66.5 - -
TiC - 6.4 17.6 12.6 12.6 12.6 6.9 20.4 8.8 - -
b.粉體中之Si/(Si+Ti) ※SiC除外 0.400 0.488 0.417 0.453 0.453 0.453 0.493 0.416 0.488 0.396 0.396
c.燒成條件 燒成溫度 ℃ 1400 1370 1370 1400 1350 1370 1430 1400 1430 1400 1370
載重 kgf/cm2 200 200 200 200 200 200 200 200 200 200 200
d.組成相 mass% SiC 39.1 45.9 40 39.3 40.4 38.8 39.8 30.1 29.5 40.2 40.1
TiSi2 47.5 47.7 43.7 49.2 48.5 49.8 52.9 49.1 62.4 44 41.5
Ti3 SiC2 5.7 - 3.4 0.7 - 1.1 - 8.6 - 13.1 14.5
TiC 7.4 5.4 12.7 10.5 10.8 10.3 6.6 12.1 7.7 2.1 3.9
e.特性 體積密度 g/cm3 3.78 3.59 3.81 3.78 3.76 3.76 3.74 3.92 3.85 3.78 3.58
開孔孔隙度 % 0.04 0.03 0.01 0 0.1 0.04 0.03 0.01 0.02 0.06 4.14
四點抗彎強度 Mpa 336 361 288 301 275 334 297 254 250 301 239
熱膨脹係數 ppm/K 7.7 7.2 7.6 7.7 7.7 7.7 7.8 7.9 8.2 7.7 7.7
熱傳導率 W/mK 90 85 88 92 89 89 90 77 71 91.7 80
SiC粒子間距離 平均值μm 6.0 4.1 5.0 5.1 4.4 4.3 6.2 6.6 9.0 8.3 9.4
SiC粒子間距離 標準偏差 5.5 4.3 4.9 4.5 5.6 4.4 6.1 6.6 7.6 11.6 17.3
SiC粒子間距離 最大值μm 27.5 26.7 26.5 28.8 25.3 22.4 27.9 34.7 36.3 59.9 95.7
3.組成相之定量 以研缽將緻密質複合材料粉碎而形成為粉末，在2θ=5°~70°之範圍進行此粉末之XRD測定，將所得之XRD繞射圖形作為對象，進行了裏特沃爾德分析。分析軟體使用了Bruker AXS製之TOPAS。
4.基本特性之測定 (1)原料之平均粒徑 使用了堀場製作所製、LA950V2，以純水為分散介質來測定。 (2)開孔孔隙度及體積密度 以將純水作為介質之阿基米德法測定。 (3)四點抗彎強度 根據JIS-R1601求出 (4)線膨脹係數(40~570℃之平均線膨脹係數) 根據JIS-R1618求出。具體而言，使用了日本理學(Rigaku)製、Thermo plus EVO(直立型示差膨脹測定方式)，在氬氣體環境中，以升溫速度10℃/分之條件升溫二次至600℃，從第二次之測定資料算出40~570℃之平均線膨脹係數，標準試樣使用了裝置附屬之氧化鋁標準試樣(純度99.7%、體積密度3.9g/cm3 、長度20mm)。又再準備一條此氧化鋁標準試樣，以同一條件測定了線膨脹係數之值為7.7ppm/K。 (5)熱傳導率 根據JIS-R1611以雷射閃光法測定 (6)SEM觀察 進行了緻密質複合材料之SEM觀察。在SEM觀察，將緻密質複合材料之截面進行鏡面研磨，以電子顯微鏡(SEM；日本電子製JSM-IT500LA)用反射電子影像觀察。反射電子影像之觀察以加速電壓10~15kV、PC30~45之條件進行。於圖1顯示各實驗例之SEM圖像(倍率500倍)。 (7)碳化矽之粒子間距離的平均值、標準偏差及最大值 藉使用日本Roper股份有限公司製之圖像分析軟體「Image-Pro ver.9.3.2」，將圖1所示之SEM圖像進行圖像解析，而求出了碳化矽之粒子間距離。具體而言，在SEM圖像，排列了平行延伸之五條直線。各直線之寬度為0.2μm。又，該SEM圖像之一像素對應0.2μm×0.2μm。接著，自動算出在直線上與亮部(即，Ti-Si矩陣)重複之區域(以下稱為「亮區」。)之面積。此時，由於各直線配置於像素列之交界線上，故在亮區之面積算出，根據直線選取寬度0.4μm之區域(即，具有二像素量之寬度的區域)。寬度0.2μm之直線配置於在寬度方向相鄰之二列像素列(即，於與寬度方向垂直之方向排列的複數之像素列)的交界線上，與直線有重疊之所有像素為面積算出之對象。在亮區之面積算出，由於一像素(即0.04μm2 )以下之區域未被計算，故不足0.05μm2 之區域作為雜訊而無視。接著，求出亮區之面積作為碳化矽粒子間之矩陣面積。矩陣面積係碳化矽的粒子間距離與選取作為亮區之直線寬度(即，0.4μm)的乘積。因而，藉上述亮區之面積除以0.4μm，可算出碳化矽之粒子間距離。使用算出之所有粒子間距離，求出其平均值、標準偏差及最大值。
5.結果 實驗例1~9之緻密質複合材料的碳化矽之粒子間距離的最大值為40μm以下(具體為20~40μm)，標準偏差為10以下(具體為4~8)。又，碳化矽之粒子間距離的平均值為4~10μm(具體為4~9μm)。此等緻密質複合材料的開孔孔隙度為1%以下而十分緻密化，四點抗彎強度為250MPa以上而強度足夠高，熱傳導率為70W/mK以上而具有良好之熱傳導性，線膨脹係數為7.2~8.2ppm/K，與氧化鋁幾乎同等(與氧化鋁之線膨脹係數的差之絕對值為0.5ppm/K以下)。
另一方面，實驗例10之緻密質複合材料的碳化矽之粒子間距離的最大值為59.9μm，標準偏差為11.6，平均值為8.3μm，具有與實驗例1~9同等之特性(開孔孔隙度、四點抗彎強度、熱傳導率、線膨脹係數)。此視為因碳化鈦矽之含有率較高至13.1質量%之故。即，由於實驗例10之緻密質複合材料的碳化矽之粒子間距離長，其偏差亦大，故有強度降低之虞，但因高強度之碳化鈦矽分布於碳化矽之粒子間，而獲得良好之特性。然而，由於碳化鈦矽在燒結製程生成，故有其生成量或分布隨著批別的不同而產生偏差之情形，並非可一直獲得良好之特性。舉例而言，在實驗例11，原料之成分及調和比與實驗例10相同，但將燒成溫度從實驗例10之1400℃變更成1370℃。因此，開孔孔隙度大至4.14%，強度亦僅239MPa。觀看實驗例11之SEM圖像(圖1(k))，可知部分產生漆黑之處(箭頭所指之處)。此漆黑處為燒結不良部(氣孔)。相對於此，在實驗例1~9，藉改善緻密質複合材料之微構造(亦即控制碳化矽之粒子間距離)，即使不生成碳化鈦矽，亦可獲得良好之特性。故不管批別如何，皆可穩定獲得良好之特性。
6.關於接合體 於在實驗例1所得之緻密質複合材料樣本(直徑50mm、厚度8mm)依序積層鋁為主構成材料之厚度200μm的金屬箔(長、寬與前述樣本相同)、厚度5mm之緻密質氧化鋁燒結體，收納於燒成用石墨模具，在100kgf/cm2 之壓力、600℃真空下熱壓燒成。如此進行後，獲得了界面無剝離或空隙之接合體(金屬接合體)。又，使用在實驗例2及實驗例9所得之緻密質複合材料樣本取代在實驗例1所得之緻密質複合材料樣本，同樣地製作了接合體後，均是界面無剝離或空隙。 [產業上之可利用性]
本發明之緻密質複合材料用於例如金屬接合於氧化鋁製靜電吸盤或基座等之冷卻板。
本申請案以2020年1月29日提申之日本專利申請案第2020-012343號為優先權主張之基礎，其所有內容藉引用而包含在本說明書內。
圖1(a)~(k)係各實驗例之複合材料的SEM照片。

Claims (10)

  1. 一種緻密質複合材料，其含有矽化鈦43~63質量%，並且含有碳化矽及碳化鈦各少於矽化鈦之質量%，碳化矽之粒子間距離的最大值係40μm以下，標準偏差係10以下，開孔孔隙度係1%以下；碳化矽係29~46質量%，碳化鈦係5~15質量%。
  2. 如請求項1之緻密質複合材料，其中，碳化矽之粒子間距離的平均值係4~10μm。
  3. 如請求項1或請求項2之緻密質複合材料，其中，與氧化鋁之40~570℃的平均線膨脹係數之差的絕對值係0.5ppm/K以下。
  4. 如請求項1或請求項2之緻密質複合材料，其中，熱傳導率為70W/mk以上。
  5. 如請求項1或請求項2之緻密質複合材料，其中，四點抗彎強度為250MPa以上。
  6. 如請求項1或請求項2之緻密質複合材料，其含有碳化鈦矽。
  7. 一種接合體，其接合了由如請求項1至請求項6中任一項之緻密質複合材料構成的第1材與由氧化鋁構成之第2材。
  8. 如請求項7之接合體，其中，該第1材與該第2材係金屬接合。
  9. 一種半導體製造裝置用構件，其由如請求項7或請求項8之接合體構成。
  10. 一種緻密質複合材料之製法，其包含有下列製程：(a)調製一種粉體混合物，該粉體混合物含有平均粒徑為10~25μm之碳化矽24~45質量%、平均粒徑不足10μm之矽化鈦42~67質量%，並且含有平均粒徑不足20μm之金屬鈦或平均粒徑不足10μm之碳化鈦；(b)在惰性氣體環境下以熱壓使該粉體混合物以1350~1430℃燒結；在製程(a)，關於該粉體混合物之源自碳化矽以外的原料之Si及Ti，Si/(Si+Ti)之質量比係0.40~0.50。
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