TWI484000B - 半導體元件接合用的貴金屬糊狀物 - Google Patents

半導體元件接合用的貴金屬糊狀物 Download PDF

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Publication number
TWI484000B
TWI484000B TW100136012A TW100136012A TWI484000B TW I484000 B TWI484000 B TW I484000B TW 100136012 A TW100136012 A TW 100136012A TW 100136012 A TW100136012 A TW 100136012A TW I484000 B TWI484000 B TW I484000B
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Taiwan
Prior art keywords
noble metal
paste
metal paste
powder
gold
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TW100136012A
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English (en)
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TW201219505A (en
Inventor
Masayuki Miyairi
Nobuyuki Akiyama
Katsuji Inagaki
Toshinori Ogashiwa
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Tanaka Precious Metal Ind
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Publication of TW201219505A publication Critical patent/TW201219505A/zh
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Publication of TWI484000B publication Critical patent/TWI484000B/zh

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    • H—ELECTRICITY
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    • H01L24/26—Layer connectors, e.g. plate connectors, solder or adhesive layers; Manufacturing methods related thereto
    • H01L24/28—Structure, shape, material or disposition of the layer connectors prior to the connecting process
    • H01L24/29—Structure, shape, material or disposition of the layer connectors prior to the connecting process of an individual layer connector
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K1/00—Soldering, e.g. brazing, or unsoldering
    • B23K1/0008—Soldering, e.g. brazing, or unsoldering specially adapted for particular articles or work
    • B23K1/0016—Brazing of electronic components
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/02—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape
    • B23K35/0222—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by mechanical features, e.g. shape for use in soldering, brazing
    • B23K35/0244—Powders, particles or spheres; Preforms made therefrom
    • B23K35/025—Pastes, creams, slurries
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
    • B23K35/24—Selection of soldering or welding materials proper
    • B23K35/30—Selection of soldering or welding materials proper with the principal constituent melting at less than 1550 degrees C
    • B23K35/3006—Ag as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
    • B23K35/00—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting
    • B23K35/22—Rods, electrodes, materials, or media, for use in soldering, welding, or cutting characterised by the composition or nature of the material
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    • B23K35/3013—Au as the principal constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
    • B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
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    • C09K5/08—Materials not undergoing a change of physical state when used
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Description

半導體元件接合用的貴金屬糊狀物
本發明係關於適合於基板與半導體元件之接合的貴金屬糊狀物。
在半導體元件之對於基板的黏晶等，各構件之接合時，焊接材被廣泛使用，無助焊劑之焊接材之金錫系焊接材被一般得廣泛使用。使用焊接材來接合各種構件之情況，已知將透過焊接材接合之一對的構件配置後，加熱至焊接材溶融之熔點以上(約300℃)而使焊接材溶融之方法。然而，若加熱成如此高溫，接合後會由於施加於構件之熱應力，在半導體元件等構件中，有產生電氣特性變動的問題之情況。
由此理由來看，藉由儘可能低溫的加熱而可使構件接合之材料被期望取代焊接材，做為該材料，在例如專利文獻1中，記載了含有銀粉與環氧樹脂，可在100~200℃之相較低溫接合之銀糊狀物。又本發明者等，在專利文獻2中，提供具有既定的純度及粒徑之含有金粉與有機溶劑的金糊狀物。
先行專利文獻： 【專利文獻】
【專利文獻1】日本專利特開2004-359830號公報
【專利文獻2】日本專利特開2007-324523號公報
然而，如上述專利文獻1般含有樹脂之糊狀物，在接合時的加熱樹脂無法完全分解，有殘留於接合後的構件之情況。因此，在半導體晶片等之構件中，殘存的樹脂成為汙染原因，而有影響半導體性能等之情況。此點，專利文獻2之糊狀物，雖可以做成不含有樹脂之構成，但在此情況，糊狀物塗佈時貴金屬粒子之凝集有較容易進行的情況，或有機溶劑有從所塗佈的糊狀物滲出的情況，難以均一塗佈。又，在如專利文獻2之含有有機溶劑的糊狀物，加熱塗佈後的糊狀物而使金燒結時，會由於有機溶劑的揮發等而在燒結體中產生空洞的情況。
因此在本發明中，係以提供在接合部不會產生構件汙染之貴金屬糊狀物，可對接合構件均一塗佈，且由於接合時之加熱，貴金屬燒結後的燒結體之狀態也為良好之貴金屬糊狀物為目的。
本發明者們，為解決上述課題，對於不使用可能成為接合後的汙染原因之各種樹脂等，而可對接合構件均一塗佈之貴金屬進行檢討。其結果，想到如以下之本發明之貴金屬糊狀物。
亦即，本發明係關於由貴金屬粉與有機溶劑構成，貴金屬粉為純度99.9質量%以上，平均粒徑0.1~0.5μm，有機溶劑為沸點200~350℃，貴金屬糊狀物從藉由回轉黏度劑測定之在23℃中對於剪切速率40/s之黏度之4/s之黏度的測定值來算出之觸變指數(TI)值在6.0以上之半導體元件接合用的貴金屬糊狀物。本發明之貴金屬糊狀物，不含有可能成為接合構件之汙染原因的各種樹脂，對於接合構件，可濡濕性良好且均一得塗佈。又，藉由本發明之貴金屬糊狀物，可維持塗佈後之貴金屬粒子之分散性均一，因此接合時之加熱時，可均一放出由於有機系成分的揮發‧分解而形成之脫氣，而可抑制空洞的發生。
在此，說明關於在本發明之糊狀物中所規定之「TI(觸變指數)值」。在貴金屬等之糊狀物中，一般而言，隨著在測定時對於糊狀物施加之剪斷速度愈大，黏度有低下之傾向。在如此背景下，TI值係藉由剪斷速度不同之2種的回轉速度而測定之黏度的值，做為兩者之黏度的比而算出，因此，TI值係表示對於剪斷速度之黏度變化之值，亦即，表現觸變性高低的指標。
本發明之貴金屬糊狀物之TI值在6.0以上，觸變性適當的高。因此，在塗佈糊狀物時不僅可維持成形性，也可使藉由接合時的加熱之貴金屬的燒結均一進行，而可使燒成後之燒結體為緻密的狀態。由於此優點來看，本發明之貴金屬糊狀物，特別適合於進行大面積塗佈之黏晶接合。若TI值未滿6.0，則在將貴金屬糊狀物塗佈於接合構件時溶劑有滲出(Bleed out)的情況。又，做為TI值的上限值，以20以下為佳。若超過20，則在貴金屬糊狀物塗佈前之混練時有難以操作的傾向。
又，關於在算出TI值之前提的剪切速率4/s之黏度，以100~1000Pa‧s為佳。若未滿100Pa‧s，則貴金屬粉沉降而有容易與溶劑分離的傾向，若超過1000Pa‧s，則操作性容易低下。以下，對於本發明之貴金屬糊狀物詳細說明。
首先，說明構成本發明之貴金屬糊狀物之有機溶劑說明。在本發明中之有機溶劑，為沸點200~350℃(大氣壓下)之物。有機溶劑之沸點，若未滿200℃，在接合時加熱時，有機溶劑的蒸發速度快，不僅貴金屬粒子之凝集控制變得困難，且在有的情況，即使在常溫有機溶劑也會蒸發，因此糊狀物塗佈時之操作變得困難。另一方面，有機溶劑的沸點若超過350℃，則有機溶劑有殘留在接合後的構件之情況。有機溶劑，若在該沸點的範圍內，可含有1種或2種以上。在此，關於本發明，「沸點200~350℃」，係指在含有2種以上的有機溶劑之情況，所含有之全部種類的有機溶劑，沸點分別在200~350℃之範圍內的意思。
做為可在本發明利用之有機溶劑，以分枝鏈狀飽和脂肪族2價醇類、單萜烯醇類為佳，做為分枝鏈狀飽和脂肪族2價醇類，係使用丙二醇、1,2-丁二醇、1,3丁二醇、1,2-戊二醇、1,3-戊二醇1,4-戊二醇、1,5-戊二醇、2,3-戊二醇、2,4-戊二醇、1,2-己二醇、1,3-己二醇、1,4-己二醇、1,5-己二醇、1,6-己二醇或其衍生物，做為單萜烯醇，可使用香茅醇、香葉醇、橙花醇、薄荷醇、萜品醇、黃蒿醇、側柏醇、松莰醇、β-葑醇、二甲基辛醇、羥基香茅醇或是這些得衍生物。
若考慮溶劑的沸點，上述有機溶劑之碳數以5~20為佳。特別是，僅從1種有機溶劑形成之情況，以使用碳數為5~20之飽和脂肪族2價醇為佳，2,4-二乙基-1,5-戊二醇(製品名　日香MARS；日本香料藥品(股份公司)，以下記載為MARS。)特別適合。由2種有機溶劑形成的情況，以混合碳數為5~20之單環式單萜烯醇與2環式單萜烯醇使用為佳，將環己异龍腦酯(製品名TersolveMTPH；日本Terpene化學(股份公司)，以下，記載為MTPH。)與α-萜品醇以質量比1/1~3/1之比率混合之物特別適合。
接著，說明構成本發明之糊狀物之貴金屬粉。做為貴金屬粉，可使用金粉或銀粉，或是其混合粉。若考慮電氣、熱傳導性，特別適合僅使用金粉。
做為貴金屬粉之純度要求99.9質量%以上之高純度，係由於若純度低，則金粒子之燒結舉動變得不安定，而接合強度的安定性低下，或是接合後之接合構件變硬而容易由於熱衝擊等造成產生裂痕之故。又，貴金屬粉的平均粒徑為0.1~0.5μm。在超過0.5μm之粒徑的貴金屬粉，在糊狀物中之分散狀態的維持變得困難，貴金屬粉容易沉降。又，藉由接合時之加熱而燒結貴金屬粉後，也難以使貴金屬粉之間出現較佳的接近狀態。另一方面，平均粒徑若未滿0.1μm，則貴金屬粉有發生凝集的情況。
在糊狀物中貴金屬粉之含有量，以體積含有率(貴金屬粉之體積/貴金屬糊狀物全體之體積)在26~66體積%(v/v)之範圍內為佳。若為如此之體積含有率，則容易成為TI值為6.0以上之貴金屬糊狀物。又，接合後的燒結體也容易成為緻密的狀態，而可實現密著性高的接合。金屬粉的含有率，若未滿26體積%，則難以得到密著性提高的效果，糊狀物也變得難以混練。另一方面，若超過66體積%，則貴金屬粉有發生凝集的情況。貴金屬的含有量，若為35~55體積%(v/v)則更佳。
在以上所說明之由貴金屬粉與有機溶劑構成之貴金屬糊狀物中，更可含有0.05~1質量%之界面活性劑。若含有界面活性劑，則在貴金屬糊狀物中，貴金屬粉容易維持均一擴散之狀態。界面活性劑若未滿0.05質量%則貴金屬粉之凝集抑制效果低，若超過1質量%則界面活性劑有殘留在接合後之構件的情況。做為界面活性劑，以陽離子性界面活性劑為佳，例如可使用十二烷基三甲基銨鹽、十六烷基三甲基銨鹽、十八烷基三甲基銨鹽、十二烷基二甲基銨鹽、十八烷基二甲乙基銨鹽、十二烷基二甲基苄基銨鹽、十六烷基二甲基苄基銨鹽、十八烷基二甲基苄基銨鹽、三甲基苄基銨鹽、三乙基苄基銨鹽等之第4級銨鹽；十八烷基胺鹽、十八酰胺鹽、N-烷基烯烴二胺鹽等之烷基胺鹽系；十六烷基吡啶鎓鹽、十二烷基吡啶鎓鹽等之吡啶鎓鹽系。其中，又以烷基(C8-C18)胺醋酸鹽(製品名：ARMACC)、N-烷基(C14-C18)三甲撐二胺烯酸鹽(製品名：DUOMEEN TDO)特別適合。又，高分子系界面活性劑，由於分解時需要高溫，因此不適合於本發明。
如以上所說明，本發明之貴金屬糊狀物，不會產生接合後之構件汙染等，而可對各種接合構件均一塗佈，且由於接合時之加熱之燒結也可均一得進行。
以下，對於本發明之較佳的實施形態說明。
[實施例1]
將藉由濕式還原法製造之純度99.99質量%的金粉(平均粒徑：0.3μm)95質量%，與做為有機溶劑之環己异龍腦酯(MTPH)3.75質量%，與α-萜品醇1.25質量%混合而調整金糊狀物。在此金糊狀物中金粉的體積含有率為49.6體積%。對於所使用之有機溶劑及所得到之金糊狀物，進行以下物性測定。
物性測定
有機溶劑及金糊狀物之黏度，係以圓錐型回轉黏度計(HAAKE公司製，Rheostress RS75，圓錐板：鈦製35mm、φ1°、以間隙0.050mm來測定)，測定溫度23℃，以剪切速率0/s保持30秒後，分別以剪切速率4/s、20/s、40/s的順序保持30秒而連續測定。有機溶劑的沸點，係藉由TG-DTA(熱重量/示差熱同時分析：Rigaku製TG8101D)，在大氣下以10℃/min之升溫速率來測定。又觸變指數(TI)值，係從前述剪切速率4/s及40/s之黏度測定值以下述式來算出。又，對於實施例1之金糊狀物，進行了TG-DTA(熱重量/示差熱同時分析)。
TI=(剪切速率4/s的黏度)÷(剪切速率40/s的黏度)
由以上結果，實施例1之金糊狀物之剪切速率4/s的黏度為256Pa‧s。又，根據TG-DTA，可確認到在實施例1之金糊狀物，在70℃有機溶劑開始蒸發，在190℃有機成分完全消失。
[實施例2~5、比較例1~7]
使用同於實施例1之金粉，以表1所示有機溶劑及金含有量來做成金糊狀物。在實施例2中，使用平均粒徑為0.1μm之金粉。在比較例7使用雙烯基琥珀醯亞胺(King Industries公司製，商品名：KX1223C)。對於各實施例及比較例，以同於實施例1之方法測定有機溶劑的黏度及沸點，與金糊狀物之黏度及TI值。結果示於表1。
由以上之物性測定結果來看，顯示實施例1~5之貴金屬糊狀物，TI值為6.0以上。相對於此，在比較例1~3、5、7，TI值為未滿6.0。又，在比較例4、6，即使將金粉與有機溶劑混合，貴金屬粉會馬上沉降而與溶劑分離，或是成為難以操作之物，皆無法糊狀化。
[金粉之平均粒徑]
以上之實施例及比較例之外，使用平均粒徑0.7μm及0.05μm之物做為金粉，同於實施例1做成金糊狀物。其結果，在金粉之平均粒徑為0.7μm之情況，糊狀物中之金粉的分散無法維持而發生沉降，0.05μm之情況，糊狀物中確認到部分的凝集。
[銀糊狀物]
又，使用銀粉(86重量%；37體積%)取代金粉，同於實施例1做成銀糊狀物，進行物性測定。其結果，所得到之銀糊狀物，剪切速率4/s的黏度為176Pa‧s，剪切速率40/s的黏度為19Pa‧s，TI值為9.3。
對於基板之塗佈試驗
接著，將上述實施例1~5及比較例1~3、5之金糊狀物，在100mm2 之半導體基板(矽)中央，使面積成為25 mm2 來塗佈，評價對於基板之塗佈性能。又，基板係使用預先在表面上濺鍍鈦(50nm)、金(200nm)而製膜之物。
上述的結果，實施例1~5的金糊狀物，具有適當的濡濕性而容易塗佈於基板，塗佈後之金糊狀物也維持充分的成形性。另一方面，比較例3之金糊狀物，有溶劑從塗佈後之金糊狀物滲出之傾向，塗佈後之糊狀物為會產生變形之物。
接合試驗
如上述塗佈糊狀物後，不進行乾燥及燒結，進行以下的接合試驗。接合試驗係在塗佈後之糊狀物上，載置面積4 mm2 之矽晶片(預先以鈦(50nm)、金(200nm)製膜)，加熱及加壓來進行。接合時的加壓，為平均每1晶片為20N(5MPa)，加熱係藉由從工具的傳熱而成為230℃，加熱及加壓時間為10分鐘。
對於藉由上述而接合之接合部，透過外觀X光透視像(Unihite-system公司製)來進行組織觀察，基於下述式算出接合率。接合率的結果示於表2。又，實施例1及比較例1之X光透視像，以及實施例1之剖面SEM觀察結果係示於第1圖。在X光透視像中，在接合部，空洞發生而產生空隙的部分觀測為白色，接合部密著的部分觀測為灰色(黑色)。
接合率={密著的部分(X光透過畫像中灰色部分)之面積}÷{接合部全體(X光透過畫像中灰色部分與白色部分的合計)的面積}
由第1圖的結果來看，藉由實施例1之金糊狀物之接合部，在外觀X光透視像中，幾乎不會觀察到由於空洞發生而造成之空隙之白色部分，在剖面SEM像中，金屬粉末也以接近於點接觸之狀態鄰接。又，在表2之接合率也在90%以上。藉由以上，可確認到由於接合時之加熱而金粉的燒結均一得進行。
使用實施例2~5之糊狀物的情況，從表2也可確認到接合率為90%以上，同於實施例1，幾乎觀察不到空洞的發生，可確認燒結均一的進行。又，使用銀糊狀物接合的情況，從外觀X光透視像，也幾乎觀察不到空洞的發生，也可確認到銀粉的燒結均一得進行。
另一方面，使用比較例1之金糊狀物之情況，從表2可確認到接合率未滿90%，在第1圖之外觀X光透視像，觀察到多數由於空洞發生而造成之空隙的白色部分。因此，在比較例1中，在接合時的加熱時，由於有機成分由來之脫氣(放出)，而發生多數的空洞，被認為金粉之燒結沒有均一得進行。
在使用比較例2、3、5之糊狀物之情況，也可從表2確認到接合率未滿90%，觀察到多數由於空洞發生而造成之空隙的白色部分。又，在使用比較例7之金糊狀物接合之情況，藉由外觀X光透視像，觀察到多數由於空洞發生而造成之空隙的白色部分。
接合強度試驗
接著，關於在以上進行之接合，遵照第2圖進行接合強度試驗。接合強度，係對於在半導體基板10上透過燒結體20而接合之半導體晶片(耐熱性矽晶片)30，從橫方向以一定速度使刀片與晶片接觸，使其行進，測定發生破斷(晶片的剝離)時之應力的平均值(單位：N)。從此測定值與破斷後之接合部面積來算出平均每單位面積之接合強度的平均值(單位：MPa)。結果示於表3。
從表3，可確認到使用實施例1~5之糊狀物接合之情況，接合部為對於電子零件之接合等為充分之接合強度(20MPa)。又，在使用比較例1之糊狀物之接合，雖然關於接合強度與實施例為相同程度，但由於如以上說明，接合率低(表2)，觀察到多數的空洞發生(第1圖)，因此並非適合於電子零件之接合。
【產業上之可利用性】
本發明之貴金屬糊狀物，適合於各種接合構件之低溫接合，在將被擔心有熱應力的影響之半導體元件等接合於基板時為有用。
10．．．半導體基板
20．．．燒結體
30．．．半導體晶片
第1圖係藉由接合部外觀X光透視像及電子顯微鏡(SEM)之剖面觀察結果。
第2圖係表示接合強度之試驗方法之圖。

Claims (5)

  1. 一種半導體元件接合用的貴金屬糊狀物，係在由貴金屬粉與有機溶劑構成之貴金屬糊狀物中，貴金屬粉為純度99.9質量%以上，平均粒徑0.1~0.5μm，有機溶劑為沸點200~350℃，其特徵在於，貴金屬糊狀物從藉由回轉黏度劑測定之在23℃中對於剪切速率40/s之黏度之4/s之黏度的測定值來算出之觸變指數(TI)值在6.0以上。
  2. 如申請專利範圍第1項之貴金屬糊狀物，其中，貴金屬粉為金粉或銀粉之任一種以上形成。
  3. 如申請專利範圍第1或2項之貴金屬糊狀物，其中，貴金屬糊狀物中貴金屬粉之體積含有率為26~66體積%(v/v)。
  4. 如申請專利範圍第1或2項之貴金屬糊狀物，其中，係用於半導體元件黏晶接合用。
  5. 如申請專利範圍第1或2項之貴金屬糊狀物，其中，在接合半導體元件之情況的接合部，在X光透視像中，藉由對於接合部全體的面積之接合部中密著的部分的面積的比率算出之接合率為90%以上。
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JP2023109448A (ja) 2022-01-27 2023-08-08 田中貴金属工業株式会社 ディップコーティングに好適な金ペースト及び該金ペーストを用いるディップコーティング方法
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