TWI600634B - 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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TWI600634B
TWI600634B TW103108320A TW103108320A TWI600634B TW I600634 B TWI600634 B TW I600634B TW 103108320 A TW103108320 A TW 103108320A TW 103108320 A TW103108320 A TW 103108320A TW I600634 B TWI600634 B TW I600634B
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composite material
mass
dense composite
carbide
sic
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TW103108320A
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TW201505999A (zh
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神藤明日美
井上勝弘
勝田祐司
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日本碍子股份有限公司
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
    • H01L21/67005—Apparatus not specifically provided for elsewhere
    • H01L21/67011—Apparatus for manufacture or treatment
    • H01L21/67098—Apparatus for thermal treatment
    • H01L21/67109—Apparatus for thermal treatment mainly by convection
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21D—WORKING OR PROCESSING OF SHEET METAL OR METAL TUBES, RODS OR PROFILES WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
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    • B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
    • B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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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。
於半導體製程會高溫化的靜電吸盤，為散熱有接合冷卻板。此時，有使用氧化鋁作為靜電吸盤的材料，鋁作為冷卻板的材料，樹脂作為接合材之情形。氮化鋁與鋁的線熱膨脹係數差非常大，例如氮化鋁的線熱膨脹係數為5.0ppm/K(RT-800℃：內田老鶴圃「陶瓷的物理」)、鋁的線熱膨脹係數為31.1ppm/K(RT-800℃：日本熱物性學會編，「新編熱物性手冊」)。以如此之靜電吸盤，由於使用柔軟的樹脂作為接合材，故可緩和該線熱膨脹係數差所產生的應力。
[先前技術文獻] [專利文獻]
[專利文獻1]日本特開2006-143580號公報
於上述靜電吸盤，使用樹脂作為接合材料，但樹脂由於係有機材料，故放熱性低，而容易高溫分解。因此，一般難以使用於高溫製程。由此，金屬接合已被確認，可有效地作為高散熱的接合材取代樹脂。如此以金屬接合的方法，稱為金屬接合。金屬接合的接合材，已知有例如鋁等。
但是，由於金屬接合的接合材，即金屬並無如樹脂之柔軟性，而無法緩和靜電吸盤與冷卻板之間的線熱膨脹係數差所產生的應力。由此情形，期望開發適於靜電吸盤與金屬接合的冷卻板材料，即，與氮化鋁的線熱膨脹係數差小，且具備作為冷卻板所需的特性的新材料。作為冷卻板所需的特性，可舉為維持放熱性而熱傳導係數高，為通冷卻液而緻密性高，為可耐於加工等而強度高等。
本發明係為解決如此之課題而完成者，以提供與氮化鋁的線熱膨脹係數差極小，熱傳導係數、緻密性及強度充分高的材料為主要目標。
本發明者們，調查以SiC為基礎，將TiC與TiSi2或TiC與Si的混合粉末成形後，藉由熱壓鍛燒所得之各種複合材料的基本特性，結果發現可得與氮化鋁的線熱膨脹係數差極小，熱傳導係數、緻密性及強度充分高者，而達至完成本發明。
即，本發明之緻密質複合材料，係含量最多的前 三者為碳化矽、碳化鈦矽、碳化鈦，此排列順序係表示由含量多至少的順序，包含碳化矽51~68質量%，不含有矽化鈦，而開孔率為1%以下者。
本發明的接合體，係將由如此之緻密質複合材料所組成之第1板材，與氮化鋁所組成之第2板材接合者，本發明的半導體製造裝置用構件係利用如此之接合體者。
本發明的緻密質複合材料，與氮化鋁的線熱膨脹係數差極小，熱傳導係數、緻密性及強度充分高。因此，將由如此的緻密質複合材料所組成的第1板材與氮化鋁所組成的第2板材接合的接合體，可利用於作為半導體製造裝置用構件，即使在低溫與高溫之間反覆使用，第1構件與第2構件並不會剝離，可使耐用期間變長。
第1圖係實驗例5所得之緻密質複合材料之SEM影像(反射電子像)。
第2圖係實驗例5所得之緻密質複合材料之XRD圖譜。
第3圖係實驗例15所得之緻密質複合材料之SEM影像(反射電子像)。
第4圖係實驗例15所得之緻密質複合材料之XRD圖譜。
本發明的緻密質複合材料，含量較多的前三者為碳化矽、碳化鈦矽、碳化鈦，此排列順序係表示由含量多至少 的順序，包含碳化矽51~68質量%，不含有矽化鈦，而開孔率為1%以下者。在此，含量，係根據X射線繞射的波峰所求得之值。此外，開孔率係以純水作為媒體之阿基米德法所測定之值。
本發明的緻密質複合材料含有51~68質量%碳化矽。僅含有未滿51質量%時，由於與氮化鋁的熱膨脹係數差會變大而不佳。此外，超過68質量%，則開孔率會變大或強度無法變得充分高而不佳。
本發明的緻密質複合材料含有較碳化矽少量的碳化鈦矽，含有較碳化鈦矽少量的碳化鈦。碳化鈦矽，以Ti3SiC2(TSC)為佳，碳化鈦以TiC為佳。例如，含有27~40質量%碳化鈦矽，含有4~12質量%碳化鈦為佳。
碳化矽係粒子狀態，於該碳化矽的粒子相互之間隙，碳化鈦矽及碳化鈦之至少1種，以包覆碳化矽粒子表面地存在為佳。碳化矽粒子，以高頻度分散時，容易在碳化矽粒子之間殘存氣孔，但如上所述地碳化矽粒子表面以其他的粒子包覆，則容易將該氣孔填埋，而容易成為緻密且高強度的材料而佳。
本發明的緻密質複合材料，線熱膨脹係數與氮化鋁同程度。因此，以本發明的緻密質複合材料所製作的構件與氮化鋁製作的構件接合(例如金屬接合)時，即使於低溫與高溫之間反覆使用，亦不容易剝離。具體而言，本發明的緻密質複合材料與氮化鋁於40~570℃之平均線熱膨脹係數差，以0.5ppm/K以下為佳。此外，本發明的緻密質複合材料於40~570 ℃的平均線熱膨脹係數，以5.4~6.0ppm/K更佳。再者，以與本發明的緻密質複合材料相同的條件，測定對氮化鋁添加5重量%Y2O3燒結助劑的氮化鋁燒結體於40~570℃的平均線熱膨脹係數的結果為5.7ppm/K，測定沒有燒結助劑的氮化鋁燒結體的平均線熱膨脹係數的結果為5.2ppm/K。因此，本發明係以提供，以二者之間的值之線熱膨脹係數5.5ppm/K(40~570℃)為中心值，平均線熱膨脹係數差為0.5ppm/K以下的氮化鋁燒結體為目標。
本發明的緻密質複合材料，雖熱傳導性優良，惟具體的熱傳導係數以100W/mK以上為佳。如此，則將以本發明的緻密質複合材料所製作的構件與以氮化鋁製作的構件金屬接合時，可特別有效地將氮化鋁所具有熱釋放。
本發明的緻密質複合材料，雖強度優良，惟具體的4點抗彎強度以300MPa以上為佳。如果，則容易將以本發明的緻密質複合材料所製作的構件適用於冷卻板等。
本發明之接合體，係將以上述緻密質複合材料所製作的第1板材，與氮化鋁所製作的第2板材接合(例如金屬接合)者。如此之接合體，例如可適用於半導體製造裝置用構件。半導體製造裝置用構件，可舉例如，將以上述緻密質複合材料所製作的冷卻板(第1構件)，與以氮化鋁所製作的靜電吸盤(第2構件)，以鋁或其合金為主成分之接合材接合者等。第1構件，由於與氮化鋁的線熱膨脹係數差極小，故即使在低溫與高溫反覆使用，亦不容易由第2構件剝離。此外，第1構件，由於熱傳導係數充分高，故可有效地冷卻以氮化鋁製作的第2 構件。再者，由於第1構件，緻密性充分高，故可使冷卻液通過內部，可更佳提升冷卻效率。再者，第1構件，由於強度充分高，故可充分耐於製造上述半導體製造裝置用構件時之加工或接合、使用於作為構件時之溫度差所產生的應力。
本發明之緻密質複合材料的製法，例如可為包含：(a)製作含有碳化矽43~52質量%、碳化鈦33~45質量%，殘部為矽化鈦18質量%以下，及/或，矽13質量%以下的粉體混合物的步驟；及(b)藉由將上述粉體混合物，於惰性氣氛下熱壓燒結得到上述緻密質複合材料的步驟。
於步驟(a)，碳化矽的原料粉末的粒徑，並無特別限定，平均粒徑以2~35μm為佳。此外，亦可僅使用粗粒(例如，平均粒徑15~35μm)，亦可僅使用細粒(例如，平均粒徑2~10μm)，亦可將粗粒與細粒混合使用。SiC的平均粒徑，較2μm小時，以原料中的SiC比較多的組成，則由於SiC粒子的表面積會增加而降低燒結性，難以得到緻密的燒結體。另一方面，SiC的平均粒徑較35μm大時，於燒結性沒有問題，但有降低強度之虞。此外，於步驟(a)，如上所述，亦可使用碳化矽、碳化鈦、矽化鈦作為原料粉末，惟亦可由碳化矽、碳化鈦、矽化鈦、鈦、矽之中適宜選擇使用。
於步驟(b)，所謂惰性氣氛，可舉例如，真空氣氛、氮氣氣氛、氬氣氣氛等。此外，熱壓條件，只要可得上述緻密質複合材料地設定即可。例如，熱壓時的壓力，以100~400kgf/cm2為佳，以200~300kgf/cm2更佳。熱壓時的溫度，以1550~1800℃為佳，以1600~1750℃更佳。壓力與溫度 的關係，可根據粉體混合物的組成或原料粉的粒徑等，於該範圍內適宜設定即可。例如，粉體混合物中的碳化矽的含有率低時，由於粉體混合物容易燒結，故可以相對較溫和的熱壓條件緻密化。另一方面，粉體混合物中的碳化矽的含有率高時，由於粉體混合物不容易燒結，故需以相對較嚴酷的熱壓條件緻密化。此外，碳化矽僅使用粗粒時，需用相對較嚴酷的熱壓條件緻密化，但使用混合粗粒與細粒時，可以相對較溫和的熱壓條件緻密化。再者，鍛燒時間，只要按照熱壓條件適宜設定即可，例如於1~10小時的時間適宜設定即可。但是，與僅使用粗粒時相比，使用混合粗粒與細粒時，由於可以較溫和的熱壓條件緻密化的傾向而佳。
步驟(b)之熱壓機條件，例如，粉體混合物中的碳化矽為43質量%以上未滿47質量%時，不論碳化矽為粗粒或細粒，以1600~1800℃、200~400kgf/cm2的條件為佳。此外，粉體混合物中的碳化矽為47質量%以上52質量%以下時，不論碳化矽為粗粒或細粒，以1650~1800℃、300~400kgf/cm2的條件或1750~1800℃、250~400kgf/cm2的條件為佳，碳化矽為粗粒與細粒的混合粒，則以1650~1800℃、300~400kgf/cm2的條件或1700~1800℃、250~400kgf/cm2的條件為佳。
[實施例]
以下，說明本發明之較佳的適用例。SiC原料，使用純度為96.0%以上，平均粒徑32.3μm、16.4μm或2.9μm的市售品。TiC原料，使用純度為94.5%以上，平均粒徑4.3μm的市售品。TiSi2原料，使用純度96.0%以上，平均粒徑6.9μm 的市售品。Si原料，使用純度為97.0%以上，平均粒徑2.1μm的市售品。
1.製造程序
．調配
將SiC原料、TiC原料及TiSi2原料，或SiC原料、TiC原料及Si原料，以第1、2表所示質量%秤量，以異丙醇為溶劑，於尼龍製的罐子，以直徑10mm的鐵芯尼龍球，濕式混合4小時。取出混合後的漿料，於氮氣流中以110℃乾燥。之後，通過30網目的篩網，作成調配粉末。再者，將秤量之原料約300g投入高速流動混合機(粉體投入部的容量1.8L)，以攪拌翼的旋轉數1500rpm混合時，確認可得與濕式混合相同的材料特性。
．成形
將調配粉末，以200kgf/cm2的壓力單軸加壓成形，製作直徑50mm、厚度15mm程度的圓盤狀成形體，收納於鍛燒用石墨模。
．鍛燒
藉由將圓盤狀成形體，熱壓鍛燒得到緻密質燒結材料。於熱壓鍛燒，於真空氣氛以第1、2表所示鍛燒溫度(最高溫度)及壓製壓力鍛燒，至鍛燒結束。於鍛燒溫度的持溫時間為4小時。再者，以下，將熱壓略稱為HP。
2.各實驗例
於第1、2表表示，各實驗例之出發原料組成(質量%)、SiC原料的粒徑與其比例、HP鍛燒條件、由XRD測定結果求得之燒結體的構成相與其量比(簡易定量結果)、燒結體的基本特性 (開孔率、體積密度、4點抗彎強度、線熱膨脹係數、熱傳導係數)。再者，實驗例1~36之中，實驗例3~7、10、12、13、15、16、18~21、23、24、26、33~36相當於本發明之實施例，剩下的實驗例相當於比較例。
3.構成相的簡易定量
將複合材料以研缽粉碎，藉由X射線繞射裝置鑑定結晶相。測定條件CuKα、40kV、40mA、2θ=5~70°、使用封入管式X射線繞射裝置(BLUKER AXS製D8 ADVANCE)。此外，進行構成相的簡易定量。該簡易定量，係基於X射線繞射的波頂要得含於複合材料的結晶相的含量。在此，分成SiC、TSC(Ti3SiC2)、TiC及TiSi2進行簡易定量求得含量。於簡易定量，利用BLUKER AXS公司之粉末繞射數據分析用軟體「EVA」的簡易輪廓擬合功能(FP MEval.)。本功能係使用定性的結晶相的ICDD PDF卡的I/Icor(對剛玉的繞射強度的強度比)算出構成相的量比者。各結晶相的PDF卡號，係使用SiC：00-049-1428、TSC：01-070-6397、TiC：01-070-9258(TiC0.62)、TiSi2：01-071-0187。再者，第1、2表中「-」係表示於XRD圖譜無法檢出該相。
4.基本特性的測定
(1)開孔率及體積密度
以純水作為媒體藉由阿基米德法測定。
(2)4點抗彎強度
遵照JIS-1601求得。
(3)線熱膨脹係數(40~570℃的平均線熱膨脹係數)
使用BLUKER AXS(股)製，TD5020S(臥式示差膨脹測定模式)，於氬氣氛中，以升溫速度20℃/分鐘的條件，升溫至650℃ 2次，由第2次的測定數據算出40~570℃的平均線熱膨脹係數。於標準試片使用裝置附屬的氧化鋁標準試片(純度 99.7%，體積密度3.9g/cm3，長度20mm)。另外準備1支該氧化鋁標準試片，以相同條件測定之線熱膨脹係數之值7.7ppm/K。再者，於本條件，測定對氮化鋁添加5重量%Y2O3燒結助劑的氮化鋁燒結體於40~570℃的平均線熱膨脹係數的結果為5.7ppm/K，測定沒有燒結助劑的氮化鋁燒結體的平均線熱膨脹係數的結果為5.2ppm/K。
(4)熱傳導係數
以雷射閃光法測定。
5.結果
(1)實驗例1、2
於實驗例1，使用平均粒徑為16.4μm的SiC原料，於實驗例2，使用平均粒徑為2.9μm的SiC原料以外，以相同原料組成，相同HP鍛燒條件鍛燒。調配粉末中的SiC含有率為41.2質量%。結果，於實驗例1、2，雖得到開孔率為0%的緻密質複合材料，但氮化鋁的熱膨脹係數差超過0.5ppm/K。於實驗例1、2，可認為由於使用的SiC原料過少，故所得緻密質複合材料中的SiC為50.1質量%及47.9質量%而變得過低，而熱膨脹係數沒有變得充分的低。
(2)實驗例3~6
於實驗例3~5，使用不同的HP鍛燒條件鍛燒以外，使用平均粒徑為16.4μm的SiC原料以外，將相同原料組成的調配粉末鍛燒。調配粉末中的SiC含有率為43.1質量%。結果，於實驗例3~5，得到SiC含有率為51~53質量%，開孔率為0%，熱膨脹係數分別為6.0ppm/K、6.0ppm/K及5.9ppm/K的緻密質複合 材料。該等的4點抗彎強度為300MPa以上，熱傳導係數為100W/m．K以上。此外，於實驗例6，使用平均粒徑為2.9μm的SiC原料以外，以與實驗例5相同的組成，相同HP鍛燒條件鍛燒。結果，於實驗例6，得到具有與實驗例5同等性能的緻密質複合材料。在此，將作為代表例以實驗例5所得之緻密質複合材料的SEM影像(反射電子像)與XRD圖譜分別示於第1圖及第2圖。由第1圖，可知於SiC粒子的表面至少以TSC及TiC之至少1種包覆。再者，關於其他的實驗例，亦得到同樣的SEM影像與XRD圖譜。
(3)實驗例7~12
於實驗例7~12，使用不同的HP鍛燒條件鍛燒以外，使用平均粒徑為16.4μm的SiC原料以外，將相同原料組成的調配粉末鍛燒。調配粉末中的SiC含有率為49.2質量%。結果，於實驗例7、10、12，得到SiC含有率為59~64質量%，開孔率為0.2~0.9%，熱膨脹係數為5.8ppm/K的緻密質複合材料。該等的4點抗彎強度為300MPa以上，熱傳導係數為100W/m．K以上。另一方面，於實驗例8、9、11，雖得到熱膨脹係數為5.8ppm/K的複合材料，但開孔率超過1%。於實驗例8、9，可認為雖以溫度1700℃作為HP鍛燒條件，於實驗例11，採用溫度1750℃作為HP鍛燒條件，但均壓製壓力不足，而開孔率變大。再者，關於實驗例7、10、12，亦得到與第1圖及第2圖同樣的SEM圖像及XRD圖譜。
(4)實驗例13~18
於實驗例13~18，使用不同的HP鍛燒條件鍛燒以外，使 用將平均粒徑為16.4μm的SiC原料與平均粒徑為2.9μm的SiC原料，以65：35(質量比)混合的SiC，將相同原料組成的調配粉末鍛燒。調配粉末中的SiC含有率為49.2質量%。結果，於實驗例13、15、16、18，得到SiC含有率分別為62.9質量%、65.4質量%、65.2質量%及60.9質量%，開孔率為0~0.9%，熱膨脹係數為5.7~5.8ppm/K的緻密質複合材料。該等的4點抗彎強度為300MPa以上，熱傳導係數為100W/mK以上。另一方面，於實驗例14、17，雖得到熱膨脹係數為5.7~5.8ppm/K的複合材料，但開孔率超過1%。於實驗例14，可認為雖以溫度1700℃作為HP鍛燒條件，於實驗例17，採用溫度1725℃作為HP鍛燒條件，但均壓製壓力不足，而開孔率變大。在此，將作為代表例以實驗例15所得之緻密質複合材料的SEM影像(反射電子像)與XRD圖譜分別示於第3圖及第4圖。由第3圖，可知SiC粒子的表面至少以TSC及TiC之至少1種包覆。再者，關於實驗例13、16、18亦得到與第3圖及第4圖同樣的SEM影像與XRD圖譜。
在此，對比實驗例15與實驗例9，則相對於實驗例15使用混雜粗粒與細粒的SiC原料，實驗例9使用只有粗粒的SiC原料之處不同，但除此之外，以相同的原料組成，相同的HP鍛燒條件，將調配粉末鍛燒。結果，實驗例9的燒結體並沒有充分緻密化(開孔率1.9%)，但實驗例15的燒結體有充分緻密化(開孔率為0.4%)。由此結果，可說使用混雜粗粒與細粒的SiC原料，較僅使用粗粒的SiC原料之情形，有較容易緻密化的傾向。
(5)實驗例19、20
於實驗例19、20，使用不同的SiC原料以外，將相同的原料組成的調配粉末，以相同的HP鍛燒條件鍛燒。於實驗例19，使用將平均粒徑為32.3μm的SiC原料與平均粒徑為2.9μm的SiC原料，以65：35(質量比)混合之SiC，於實驗例20，使用將平均粒徑32.3μm的SiC原料與平均粒徑為2.9μm的SiC原料，以55：45(質量比)混合之SiC。調配粉末中的SiC含有率為49.2質量%。結果，得到SiC含有率為64~66質量%，開孔率為0.5~0.8%，熱膨脹係數為5.7~5.8ppm/K的緻密質複合材料。4點抗彎強度為300MPa以上，熱傳導係數為100W/mK以上。再者，關於實驗例19、20，亦得到與第3圖及第4圖同樣的SEM影像及XRD圖譜。
在此，對比實驗例17與實驗例19，則相對於實驗例17使用平均粒徑為16.4μm的SiC原料，實驗例19使用平均粒徑為32.3μm的SiC原料之處不同，但除此之外，以相同的原料組成，相同的HP鍛燒條件，將調配粉末鍛燒。結果，實驗例17的燒結體並沒有充分緻密化(開孔率1.7%)，但實驗例19的燒結體有充分緻密化(開孔率為0.8%)。由此結果，可說使用平均粒徑較大的粗粒的SiC原料，較使用平均粒徑小的粗粒的SiC原料之情形，有較容易緻密化的傾向。特別是在SiC原料的量較多時，使粗粒的SiC量的比例較多對緻密化有效。
(6)實驗例21~26
於實驗例21~26，以不同的HP鍛燒條件緞燒以外，使用將平均粒徑16.4μm的SiC原料與平均粒徑2.9μm的SiC原料， 以65：35(質量比)混合的SiC，將相同原料組成的調配粉末鍛燒。調配粉末中的SiC含有率為51.4質量%。結果，實驗例21、23、24、26，得到SiC含有率為66~68質量%，開孔率0.2~0.9%，熱膨脹係數為5.4~5.5ppm/K的緻密質複合材料。4點抗彎強度為300MPa以上，熱傳導係數為100W/mK以上。另一方面，於實驗例22、25，雖得到熱膨脹係數為5.5ppm/K的複合材料，但開孔率超過1%。於實驗例22，可認為雖以溫度1700℃作為HP鍛燒條件，於實驗例25，採用溫度1750℃作為HP鍛燒條件，但均壓製壓力不足，而開孔率變大。再者，關於實驗例21、23、24、26，亦得到與第第3圖及第4圖同樣的SEM圖像及XRD圖譜。
(7)實驗例27~32
於實驗例27~32，使用不同的HP鍛燒條件鍛燒以外，使用將平均粒徑為16.4μm的SiC原料與平均粒徑為2.9μm的SiC原料，以65：35(質量比)混合之SiC，將相同原料組成的調配粉末鍛燒。調配粉末中的SiC含有率為53.8質量%。結果，於實驗例27~32，得到SiC含有率為68~72質量%，熱膨脹係數為5.2~5.3ppm/K的複合材料，但開孔率超過1%。於實驗例27~32，可認為由於使用的SiC原料過多，故即使以HP鍛燒亦無法充分燒結，而開孔率變高。
(8)實驗例33~36
於實驗例33~36，於原料不使用TiSi2，而使用TiC與Si，將平均粒徑16.4μm的SiC原料與平均粒徑2.9μm的SiC原料，以65：35(質量比)混合的SiC，將SiC：TiC：Si=43.2：44.2： 12.6(質量比)的原料組成的調配粉末，以不同的HP鍛燒條件鍛燒。結果，得到SiC含有率為61~63質量%，開孔率為0.1~0.9%，熱膨脹係數為5.8~5.9ppm/K的緻密質複合材料。該等的4點抗彎強度為300MPa以上，熱傳導係數為100W/mK以上。
在此，對比實驗例14、17與實驗例33、34，雖原料種類與組成不同，惟其以外，以相同的HP鍛燒條件鍛燒調配粉末。結果，實驗例14、17的燒結體並未充分緻密化，但實施例33、34的燒結體有充分緻密化。實施例33、34與實施例14、17的燒結體的SiC含量同等，故可知將原料的SiC、TiSi2減量，代之藉由使用較TiSi2的平均粒徑小的TiC、Si原料調整Si、Ti、C成分量，有更容易緻密化的傾向。
(9)總結
於實施例3~7、10、12、13、15、16、18~21、23、24、26、33~36所得之緻密質複合材料，開孔率為1%以下，線熱膨脹係數幾乎與氮化鋁相同(於40~570℃為5.4~6.0ppm/K)，熱傳導係數、緻密性及強度充分高。因此，將由如此之緻密質複合材料所組成之第1板材，與氮化鋁所組成之第2板材金屬接合之半導體製造裝置用構件，即使在低溫與高溫之間反覆使用，第1板材與第2板材不會剝離，故耐用期間會變長。由該等實驗例(相當於實施例)，可知關於得到緻密質複合材料的調配粉末，SiC在43~52質量%、TiC在33~45質量%、TiSi2在14~18質量%的範圍，關於緻密質複合材料，SiC在51~68質量%，TSC在27~40質量%，TiC在4~12質量%的範圍。此外， 由實驗例33~36的結果，將SiC、TiSi2原料的一部分或者將全量以如TiC、Si等的原料代替，亦可顯現具有同等特性之緻密質複合材料。此時，關於調配粉末，SiC在43~52質量%，碳化鈦在33~45質量%的範圍，殘部為矽化鈦在18質量%以下，及/或，Si在13質量%以下的範圍。
6.關於接合體
(1)將實驗例18所得之緻密質複合材料樣品(直徑50mm、厚度8mm)，依序積層以鋁製之厚度200μm的金屬箔(直徑與前出之樣品相同)、厚度8mm的緻密質氧化鋁燒結體(直徑與前出之樣品相同)，收納於鍛燒用石墨模具，以100kgf/cm2的壓力，於真空下以600℃，熱壓鍛燒。結果，得到於界面沒有剝離或空隙的接合體(金屬接合體)。
(2)將實驗例18的原料組成之調配粉末，以200Kgf/cm2的壓力單軸加壓成形，製作直徑50mm，厚度15mm程度的圓盤狀成形體。於該成形體，積層直徑50mm、厚度8mm程度的緻密質氧化鋁燒結體，收納於鍛燒用石墨模具，以250kgf/cm2的壓力，於真空下以1750℃ HP鍛燒。結果，得到於界面沒有剝離或空隙的接合體(直接接合體)。
【產業上的可利性】
本發明之緻密質複合材料，可使用於例如，金屬接合於氮化鋁製的靜電吸盤或晶舟等的冷卻板。

Claims (10)

  1. 一種緻密質複合材料，含量最多的前三者為碳化矽、碳化鈦矽、碳化鈦，此排列順序係表示由含量多至少的順序，包含上述碳化矽51~68質量%，不含有矽化鈦，而開孔率為1%以下者。
  2. 根據申請專利範圍第1項之緻密質複合材料，其中包含上述碳化鈦矽27~40質量%，上述碳化鈦4~12質量%。
  3. 根據申請專利範圍第1或2項之緻密質複合材料，其中上述碳化矽係粒子狀態，於上述碳化矽的粒子相互之間隙，上述碳化鈦矽及上述碳化鈦之至少1種，以包覆碳化矽粒子表面地存在。
  4. 根據申請專利範圍第1項之緻密質複合材料，其中與氮化鋁於40℃~570℃之平均線熱膨脹係數差在0.5ppm/K以下。
  5. 根據申請專利範圍第1項之緻密質複合材料，其中於40℃~570℃的平均線熱膨脹係數為5.4~6.0ppm/K。
  6. 根據申請專利範圍第1項之緻密質複合材料，其中熱傳導係數為100W/mK以上，4點抗彎強度為300MPa以上。
  7. 一種接合體，將申請專利範圍第1至6項中任一項之緻密質複合材料所構成之第1板材，與氮化鋁所構成之第2板材接合者。
  8. 根據申請專利範圍第7項之接合體，其中上述第1板材與上述第2板材係以金屬接合。
  9. 一種半導體製造裝置用構件，由申請專利範圍第7或8項之接合體所製作。
  10. 一種緻密質複合材料的製法，包含：(a)製作含有碳化矽43~52質量%、碳化鈦33~45質量%，殘部為矽化鈦18質量%以下，及/或，矽13質量%以下的粉體混合物的步驟；及(b)藉由將上述粉體混合物，於惰性氣氛下熱壓燒結得到申請專利範圍第1至6項中任一項之緻密質複合材料的步驟，其中進行上述熱壓燒結步驟時的壓力為100~400kgf/cm2，進行上述熱壓燒結步驟時的溫度為1550~1800℃，進行上述熱壓燒結步驟的時間為1~10小時。
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