TWI267498B - Aluminum nitride conjugate body and method of producing the same - Google Patents

Aluminum nitride conjugate body and method of producing the same Download PDF

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Publication number
TWI267498B
TWI267498B TW93116803A TW93116803A TWI267498B TW I267498 B TWI267498 B TW I267498B TW 93116803 A TW93116803 A TW 93116803A TW 93116803 A TW93116803 A TW 93116803A TW I267498 B TWI267498 B TW I267498B
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Taiwan
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joint
metal layer
joined
sintered body
length
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TW93116803A
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English (en)
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TW200503984A (en
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Tatsuo Esaki
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Tokuyama Corp
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    • Y10T29/49002—Electrical device making
    • Y10T29/49117—Conductor or circuit manufacturing
    • Y10T29/49124—On flat or curved insulated base, e.g., printed circuit, etc.
    • Y10T29/4913—Assembling to base an electrical component, e.g., capacitor, etc.
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T29/00—Metal working
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    • Y10T29/49826—Assembling or joining
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
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    • Y10T29/49947—Assembling or joining by applying separate fastener
    • Y10T29/49966—Assembling or joining by applying separate fastener with supplemental joining
    • Y10T29/49968—Metal fusion joining
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T29/00—Metal working
    • Y10T29/49—Method of mechanical manufacture
    • Y10T29/49826—Assembling or joining
    • Y10T29/49947—Assembling or joining by applying separate fastener
    • Y10T29/49966—Assembling or joining by applying separate fastener with supplemental joining
    • Y10T29/4997—At least one part nonmetallic
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12347—Plural layers discontinuously bonded [e.g., spot-weld, mechanical fastener, etc.]
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/12—All metal or with adjacent metals
    • Y10T428/12493—Composite; i.e., plural, adjacent, spatially distinct metal components [e.g., layers, joint, etc.]
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    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
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    • Y10T428/00—Stock material or miscellaneous articles
    • Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
    • Y10T428/24802—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.]
    • Y10T428/24917—Discontinuous or differential coating, impregnation or bond [e.g., artwork, printing, retouched photograph, etc.] including metal layer
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1267498 坎、發明說明： 【發明所屬之技術領域】 本發明係關於一種氮化鋁接合體，其在半導體製造裝 置中，可有效地當作用以載放半導體晶圓進行處理之平板 加熱器或是靜電夾。更詳細地說，係關於一種氮化鋁接合 _ /、/、有以2片氮化铭燒結體板夾住金屬層做接合之接 合構造，特別可均勻進行半導體晶圓之處理，且耐久性也 良好。 L先1T技術】 、在對方;矽晶圓等半導體晶圓施行附膜或蝕刻處理 半導體製造裝詈φ 中做為载放該半導體晶圓之台方面，係 或電Γ乍用之内部埋設有金屬層之鳴 哭 版$ ϋ，埋設有金屬層之加熱器係當作平板加埶 二：有電極者係當作靜電夹使用。又，在靜電： 忪除了電極以外也會埋設做為加熱器之金屬層。 近年來’在上述用途所使 使用熱傳導率良使用之陶竞方面，係逐漸開始 民好之虱化鋁燒結體。 另一方面，说扛十 .,^ 年來之技術革新所導致之高集積化，乃 更加需要高精度化， 门木槓化乃 ，例如，在進=者1處理之半導體晶圓也大型化 導體晶圓表面以、:：朕之處理中’需要在大面積之半 蝕刻處理中，需要：：衣作出均-、均質的薄膜，又，在 各種薄膜進行约 方、在半導體晶圓上所形成之大面積的 疋叮叼一的蝕刻。 在這種狀況了，前述做為平板加熱器或靜電夾使用之 1267498 氮化鋁板狀燒結體中所埋設之金屬層對於該燒結體上所載 放之半導體晶圓必須以均一的厚度存在。 在埋設有金屬層之氮化鋁板狀燒結體之製造方法上， 係嘗試製作出埋設有金屬層之氮化鋁製生μ，然後將此生 胚加以燒成之方法，但是在此方法中，會因為燒結時之尺 寸變化而出現金肩層之斷線或變形之問題。是以，一般所 知用之方 >去’係先製作出板狀或片狀之燒結體，然後將兩 個燒結體透過金屬層做接合。亦即，以此方法所得之氮化 鋁板狀燒、结體係兩片氮化鋁燒結中間夾設金屬層做接合 而成之接合體，可有效避免上述因燒結時尺寸變化所造成 之問題。 另—方面，以接合法來製造氮化鋁接合體時，在兩片 的燒結體板的接合中係使用接著劑。但是，以往所使用之 :接著劑，接著溫度高，且會因為接合時之加熱造成燒結 體板，變形’從而導致金屬層出現翹曲，此為問題所在。 疋以，有人提出使用接著溫度較低之接著劑來改善趣 曲之方法（參見專利文獻丨）。 猎由上述方法，接合體内之金屬層的翹 ::::良’但是仍有改良的空間。η氮二:: 可確保充分的接合強度，但是氣化銘燒結板彼此 <部分的接合強度則會因為熱經歷而隨時間的經 匕下卜’此為問題所在。 2000-252045 號公報 [專利文獻1]特開 1267498 【發明内容】 疋^本發明之目的在於择媒播4立 片氮化紹燒”拓…。于一種接合體’其可將兩 H豆板之間夾設金屬層入 合體令之内部全屬；ΑΓ_ 接5而成之氮化鋁接 強度。 "蜀層的靖抑到最低，且具有高的接合 t發明者為了解、、灰Ρ 現，若_ /N a课喊做了不斷的研究。結果發 見右虱化鋁燒結體板之接合係在施胜A 溫度控制下以9段飞進… 特』力、特定的 成功得到… 則即使不使用接著劑仍可 有而接合強度且内部金屬層之翹曲可顯著麼低 之氮t 名呂接$ 4/ 行角m 上述方法所得之接合體進 午、、、、’。果，發現在氮化鋁燒結體之接合界面，會特徵 性地殘存著起源於本方法之微細大小的空孔，從而完成了 本發明。 …亦即’依據本發明，可提供-種氮化銘接合體（以下也 稱為A1N板狀接合體），係由··在不使用接著劑之情況下 相互接合之兩片氮化鋁燒結體板、在其接合界面之一部分 所形成之金屬層所構成者，其特徵在於： 以通過該接合體中心之側截面來觀看時，該接合界面 中之燒結體板彼此直接面對之直接接合區域中係存在著複 數之沿著接合界面之長度L平均為〇 5〜4 V m之空孔，且 由該空孔形成非接合部， 針對前述側截面，以下述式（1): 非接合率 Q = (X/Y)xl00 ...(1) (式中，X係以在直接接合區域所存在之空孔長度L之 1267498 合計值所表示之非接合部在接合界面方向長度；γ為存在 者空孔之直接接合區域之長度）所算出之非接合率ρ平均 起來在0·1〜〇·5%之範圍内。 又依據本發明，可提供一種氮化叙接合體之製造方 法’係由下述製程所構成者·· 準備兩片氮化鋁燒結體板之製程； 於其中-片氮化紹燒結體板之表面的一部分形成厚度 20// m以下之金屬層之製程； 將另-片氮化銘燒結體板以前述金屬層位於中間的方 式豐合在前述其中一片氮化銘燒結體板上形成積層體之製 程； 將該積層體-邊以5〜職g/cm2之屢力加塵一邊以 1㈣〜崎之溫度進行0_5〜4小時加熱之製程；以及 其次’使得前述壓力之加壓持續進行，並 ^且在购t以下之溫度將該積層體加熱2〜8小時之製程 本發明之嫌板狀接合體由於依據上述特定之接合方 :所形成之特徵性的接合界面構造，可將金屬層之麵曲程 、、兄笙丁从 > . 兒；土方、包，丨質形成電場的情 不⑥在金屬層之任—部位均能形成均-的電場。 尉久於接合時未使用接著劑’所以對於熱經歷具有 寸久陡’可期待更咼可靠性的作用。 本發明之湖板狀接合體可極有效地使用於在 Ά裝置中所使用之靜電夾、板狀加熱器上。 ' 1267498 【實施方式] 以下，依據圖式詳細說明本發 不受限於相關圖式所示者。 惟本發明並 (A1N板狀接合體） 於圖1與圖2中’本發明之細板狀接 片氮化鋁燒处俨缸 口體係具有兩 合構造，在：二二V?未使用接著劑即進行接合之接 2。又，圖中雖圖2)之—部分存在著金屬層 通孔，於貫通孔-、π乜結體板lea、“係形成有貫 s^ 、、内部填充著導體糊，成為可盥全2 通電之構造。又，士 Δ 1χτ 1 π I、至屬層2 形或正方形等反狀接合體之平面形狀通常為圓 用途中，用 金屬層2在加熱器板或靜電夹之 圖i所、4 A、加熱器等之電路圖案者，也有如 ^在的^ 密#_存在恤’也有以線狀圖案 厚度二=;係;;7、“、銅等所形成’其 。 丁、将仏為5〜15 之範圍，但並不限定 ^ l b ，金屬層2所佔之比例通常對於燒結體板l-a 之接合面為50〜90%，特佳為6〇〜8〇%程度。 合後前之氮化峨體板一係以接 個別厚度而厂子度之細板狀接合體的方式來適宜設定 _ $如，燒結體板1 -a、1 -b可為相同厚度、也可 厚度。一般而言，載放半導體晶圓側之燒結體板的 二另侧來付薄為佳’另外，以金屬層2距離一側燒 、面（載放晶圓側之表面）的深度相對於板狀接合 1267498 體全部厚度成4 O.UO%的方式來決定燒結體板 之厚度為佳。上述A1N板狀接合體之總厚度係隨用途而略 有不同’ 一般為l〜1〇〇mm。 本發明之A1N板狀接合體並不使用接著劑，在上述氮 化鋁燒結體“、1-b之間夾設金屬層2,以後述之2段： 熱來進行接合’由於採用此種方法來製造，所以具有以下 特性。 一亦即，本發明之A1N板狀接合體之接合強度可藉由雙 剪切測試機⑷Shear tes㈣所測定之剪切強度來評價，在燒 結體板間為9_5〜ll.〇kg/mm2、特別是1〇〇〜11〇1^/細2, 在燒結體板-金屬層間為2 5〜4 〇kg/mm2、特別是 3.〇〜4.0kgW。在本發明中，由於以前述高接合強度來構 成接合體，所以相較於使用接著劑所製作之接合體，與不 同材料所產生之界面少（不存在接著劑層），是以，因為反 覆之熱經歷所造成之接合強度的降低極少，此為特性所在 。附帶一提，本發明之A1N板狀接合體在歷經從Μ。。到 35(TC之升降溫熱經歷# !⑽次後之金屬層2與氮化铭燒 結體板之接合面的剪切強度相對於前述熱經歷前之剪切強 度為90%以上，此展現了極為良好之耐熱經歷特性。 又，本發明之A1N板狀接合體之最大特徵在於金屬層 2之翹曲顯著減少這一點。此種金屬| 2之翹曲(w)如圖3 所示，係在對於金屬層2呈直角的切斷面中，係對於連結 金屬層2端點之線Z(—點鏈線）與金屬層2之最大距離（r ，私m)進行測定，並與端點間之長度（τ ;切叫以下述式（2) 1267498 W(// m/l 〇mm) = (R/T)x 1 〇 ...(2) 所算出之值。本發明之A1N板狀接合體在翹曲上展現 出5〜25/zm/lOmm、特別是1〇〜2〇//m/1〇mm之優異特性。 此種優異之低翹曲特性是以往使用接著劑之ain板狀 接合體所無法達成之值，為不使用接著劑、以後述2段加 熱之特殊接合技術始能達成之值。 又，本發明之接合體，由於藉由後述之特殊的接合技 術來實現低翹曲，所以如圖2所示般，從通過接合體中心 〇之側截面來看，在接合界面p之前述燒結體板彼此直接 面對之直接接合區域中，存在著複數之沿著接合界面之平 均長度L為〇·5〜4之空孔此種特有的接合構造。亦即 ，此種空孔在直接接合區域之全體中分布著，並不存在著 長度L為5 // m以上大小之空孔，又，該空孔具有接近球 形之形狀，其沿著接合界面方向之長度L與對於接合界面 在垂直方向之長度LP的比（L/Lp)平均為〇·8〜2、特別是 〜ι·5之範圍。本發明之Α1Ν板狀接合體由於此種空孔 之存在，燒結體板丨_a與丨讣會成為部分性非接合，針對 上述側截面在任意的複數部位以下述式（1): 非接合率 Q = (X/Y)xlOO ...(1) 式中’ X係以在直接接合區域所存在之空孔長度L之 合計值所表示之非接合部之接合界面方向長度； Y為存在著空孔之直接接合區域之長度； 所异出之非接合率Q之平均值在〇·1〜0.5%之範圍内、 特佳為0.2〜0.4%之範圍内。 12 1267498 又，上述空孔之大小與非接合率等可將板狀接合體以 出現上述側截面的方式切斷，將此切斷面以電子顯微鏡觀 察來測定。
VnUN攸狀接合月且〜衣这刀次） 以下針對具有上述構造之本發明之Am板狀接合體之 製造方法說明如下。 此製造方法係事先準備Α1Ν燒結板，而在中間夾以金 屬層的狀態下將兩片Α1Ν燒結板不使用接著劑即進行加熱 接合，簡要的言兒，此加熱接合係w 2段加熱來進行為顯著 :::徵。亦即’第1段之加熱接合係在燒結體之熱膨脹相 #車乂>之低溫區域來進行，此時燒結板彼此會產生部分的 共燒結，兩片的燒結板會被暫時固定。又’接著 2 &的加4接合，係'在較第}段加熱接合更高溫區域下進 L:下在人段之加熱接合所造成之固定狀態維持的前 夕進订共燒結來形成堅固的接合部。 月'J述加熱接合若分2段進行，則部分性共择妹 進行而形成最終的接合部（ /、几…曰緩、、友 長之共燒結部之間合…“ 接接合區域)，所以成 孔#以，、“ 而接近球狀的空孔。此種空 孔係^相大小在整個接合部全體大 2 工絲成非接合部，接合界面中 — 率Q成為既定笳η& 』义武（1)表不之非接合 千乂 α兄疋乾圍内。如此般，在 進行接合，而罝右二、+、拉入 吏用接者劑的情況下 -有則述接5構造，所以本 接合體具有高接 X月之Α1Ν板狀 綱。又，由==性，且可有效抑制金屬 由方；未使用接著劑，乃不易因發生顯著的晶 13 1267498 粒移動而出現翹曲。 例如’在氮化鋁燒結體之燒結溫度附近以1段實施加 熱接合時，隨著接合的進行雖會殘存非接合部，但是接合 守接5界面擁有自由度，此在冷卻過程之相對高溫造成接 - ’I面之固疋，所以冷卻後之接合體容易產生變形，從而 2生翹曲。又，於接合時接合界面擁有自由度，也會使得 工孔之私動或變形容易發生，大的空孔會集中存在，而在 平面方向存在許多壓潰形狀（接合界面方向之長度l大）之 空孔，前述非接合率Q成為甚大之值，造成接合強度與耐 熱經歷特性之降低。 ΔΜ燒結體柘1-a、l-h之製作 方、本發明中，待加熱接合之A1N燒結體板可藉由眾知 的方法來製作，例如將A1N粉末所構成之燒成用粉末與有 機黏合劑混合調製成造粒粉末或是糊等成形用材料，將此 成形材料成形為片狀，所得之生胚進行脫黏合劑步驟，然 後進行燒成來製作。 上述燒成用粉末中可視情況添加Mg、Ca、Sr等之鹼 土類金屬之氧化物或是γ等之稀土類元素的氧化物等做為 燒結助劑。此種燒結助劑之添加量通常為丨重量％以下、 特別是0 · 5重量％以下。 又，在有機黏合劑方面，雖無特別限定，一般可使用 χκ乙烯私縮丁醛、聚曱基丙烯酸曱酯、羧基曱基纖維素、 聚乙烯毗咯烷酮1乙二醇、氧化聚乙烯、聚乙浠、聚丙 烯乙烯乙酸乙烯酯共聚物、聚笨乙烯、聚丙烯酸等。 14 1267498 此等有機黏合劑雖依據種類而不同，—般在前述燒成用粉 末每1〇〇重量份係使用0.1〜30重量份之量。 ’亦可視情況使用適宜量 乙醇等之溶劑、以及對苯 又，在成形用材料之調製上 之長鏈_等之分散劑、曱苯、 二曱酸等之增塑劑。 ”使用上述成形用材料之成形用片（生胚)之製作可依據 t >1成ί彳刀塗佈法、加壓成形法等眾知的方法來進 行0 脫黏合劑-般係將生胚於空氣中加熱至到90(rc 左右來進仃’燒成係將脫黏合劑後之生胚在惰性環境氣氛 中（例如II環境氣氛中）加熱至i〜19⑻。c之溫度來進行 。燒成時間通常只要阿基来德法所測得之相對密度成為 98%以上之程度的時間即可。 以上述方式所得之A1N燒結體板以施行磨削加工使得 表面粗度Ra⑽B 0601)成為、較佳為〇 2~〇 6 私m為適且’錯此’可提高金屬| 2與該燒結板之密合性 ’且即使不使用接著劑即進行加熱接合仍可得到充分之接 之形成 1-a、卜13之一者形成金 於上述所製作之AIN燒結體板 屬層2。 此金屬層2例如可將前述金屬材料透過既定之光罩以 離子植入等手段形成既定厚度(2〇”以下，特別是 ㈣。又，亦可將金屬材料分散於適當的有機黏合劑或有 15 1267498 jJ中成為導體糊而在燒結體板表面塗佈成既定圖案形 狀進行烘烤而形成金屬層2。 方、本發明中係將上述所製作之兩片a1n燒結體板（一 者化成有金屬I 2)以中間存在著金屬I 2的方式重合，一 、、 〇〇kg/mm (較佳為1 〇〜3〇 kg/mm2)壓力進行壓接， :邊=行2段式加熱接合。χ，此加熱接合可在大氣中或 h丨生％ i兄氣氛中（氮氣環境氣氛）之任一情況下進行，為了 防止=屬材料之氧化，在惰性環境氣氛中進行較佳。 第1段的加熱接合係以1650〜1700 °C (較佳為 1650〜l680t:)之溫度進行〇·5〜4小時消佳為卜2小時）加 熱。如先前所述般，在此階段之加熱接合，係在Am燒結 體之熱膨脹相對少之低溫區域進行，燒結體板相互產生部 刀丨生/、燒、、Ό兩片之燒結體板係被暫時固定。是以，當此 階二之加熱接合停止時，兩片燒結體板彼此接合著之區域 之剪切強度通常為1.0〜4.0kg/mm2程度相當低。 上述弟1段之加熱接合後，保持前述壓力之狀態下 ’進订第2 &之加熱’ #以得到所需之謂板狀接合體。 此時之加熱溫度係超過1 7⑽。「 i W〇〇 C而在1800〇C以下（較佳為 1750〜179GI之範圍），加熱時間係2〜8小時，較佳為η 小％。亦卩卩ilb第2段之加熱’係使得第丨段之加熱接合 所造成之固定狀態維持著而推_本^ 讨者而進步進行共燒結來形成接合 部。是以，在兩片燒結體板呈直接接合之區域中係分布著 空孔’以此種空孔來產生非接合部。然而，此種空孔係接 16 1267498 近球狀，且整， / Q位於相 a ''、目當均一之微細形狀’前述非接合率 趣曲被有效抑制著。 妾合強度’又金屬層2之 述範圍來;r」又之加熱接合中，若第1段之加熱溫度較前 嚴重的’則所得之板狀接合體中在金屬層2會發生 以該條件所m人身會有嚴重的翹曲。又， 大甚多:。體，空孔之長度比（L/LP)會較本發明 形“空;二 =接合界面之方向上的長度長之細長 降低。 妾5率Q會變得非常大，接合強度會大幅 是二二之=溫度較前述範圍來得低的情況或 1“述爾得短的情況，暫時固定會不充分 -強产午多大的空孔，非接合率Q會變大，會產生接 口強度之降低或翹曲。 护成全尸=1段之加熱時間較前述範圍來得長的情況， 形成孟屬層2之金屬會在燒結 .^ 金屬層2之分布會變得不均在接合板内之 所使用之'電夹或板狀加熱器之用途而言極為不適當。 形成ϋ二2!二:熱溫度較前述範圍來得高的情況， 心成至屬層2之金屬也會在烊紝 >八Μ β 1 在粍結體板中擴散，在接合板内 之至屬層2之分布會變得不均_。 當第2段之加熱溫度軔侖 々 季乂則述乾圍來得低的情況，共燒 結部之成長會變得不充分，盔 去侍到充分的接合強度。亦 即，在此種狀況，當'然前述非接合率Q會成為極大之值。 17 1267498 向之長度（L)以及與接合界面成垂直方向之長度（Lp)，求出 其比（L/Lp)，以其平均值來表示。 (3) 金屬層之翹^曲（W)之測定 針對A1N板狀接合體經2分割後之各截面，如圖3所 ’ 不般，測定金屬層離開連結金屬層端點之線z(一點鏈線） 之最大距離（R ; m)，並與端點間之長度（丁 ； mm)以下述 式（2)所求出之最大值當作金屬層翹曲來表示。 W(// m/l〇mm) = (R/T)x 1〇 ...(2) (4) 耐熱經歷特性 φ 將A1N板狀接合體放入熱衝擊室（艾斯佩克（股份有限）· 製造，型式TSC-103(W))，以30分鐘從25。〇升溫至35(Γ(： 之後，花30分鐘冷卻至25t，此升降溫反覆進行ι〇〇次 ，對此種熱經歷前後之接合體的接合界面剪切強度進行測 定’以下述式算出耐熱經歷特性。 耐熱經歷㈣（％)=熱經歷後之剪切強度χ】〇〇/熱經歷 前之剪切強度 實施例1 對於直徑4〇mm、厚度6mm之Am燒結板（(股份有限） 德山，SH-50, Υ2〇3: 〇·〇2重量％，表面粗度以：〇々叫 之其中一面，從外圍起算5mm寬度部分以紹製光單來覆蓋 ，藉由離子植入法以Tl: 〇.2"m，w: 之順序來進 行成膜而形成金屬層（厚度·· L2// m)。 其次，將未形成金屬層之A1N燒結板（SH-5〇)疊合於上 述形成有金屬層之燒結板上（金屬層成為内側），然後以碳 19 1267498 製試樣治具來固定，放入熱壓爐中。之後，一邊施加負荷 3 00kgf(壓力23.9kg/cm )—邊在氮氣氣流中於丨65〇。〇保持 2小時後，以升溫速度l〇°C/分鐘升溫至175(rc，保持* 小時。冷卻至室溫後，從爐内取出，得到A1N板狀接合體 · 〇 该A1N板狀接合體之製造條件以及各種特性係示於表 1、表 2 〇 又’針對此A1N板狀接合體之金屬層的輕曲…為 // m/l〇mm，接合界面之剪切強度，包含金屬層之界面為 肇 3.8kgf/mm2，不包含金屬層之界面（燒結板彼此做直接接合 之界面）為l〇kgf/mm2，再者耐熱經歷特性為ι〇〇%。又， 非接合率Q為0.2%，接合界面方向之空孔平均長度為工$ A m，空孔長度比L/Lp之平均為1.1。 實施例2 對於直徑326mm、厚度i〇mm之A1N燒結板（組成等 與實施例1相同）之其中一面的全面與實施例1同樣來形成 由Ti以及W所構成之金屬層（厚度：1.2# m)。其次，將 鲁 自金屬層中心起算半徑146mm範圍加以遮罩，而將自外圍 起算17mm寬度之金屬層（Ti/W膜）以5體積％氫敦酸/5體 積％硝酸1 : 1之混合溶液來去除。 其次，將未形成金屬層之A1N燒結板疊合於上述A1N · 燒結板上（金屬層成為内側），然後以碳製試樣治具來固定 ，放入熱壓爐中。之後，一邊施加負荷20kgf(壓力 24.0kg/crn2)—邊在氮氣氣流中於1690°C保持2小時後，以 20 1267498 升溫速度rc/分鐘升溫至m(rc，保持4小時。冷卻至室 溫後，從爐内取出，得到AIN板狀接合體。 該Am板狀接合體之製造條件以及:種特性係示 1、表 2。 又，針對此AIN板狀接合體之金屬層的龜曲％為17 ’接合界面之剪切強度，包含金屬層之界面為 3.5kgf/mm2，不包含金屬層之界面 ^ m (乂、、古板彼此做直接接人 "面）為10kgf/]W，再者耐熱經歷特性為1〇〇%。 又’非接合率Qw.2%，接合界面方向U孔平均長 度為2·4#ηι，空孔長度比L/Lp之平均為12。 、 實施例3〜5 ，僅係使用具有與實施例1相同直徑與厚度之細燒結板 僅改變加熱接合條件（保持溫度、保持時間、負荷），除 匕以外係以與實施例1相同之方法. 。 』（万去末付到A1N板狀接合體 該A1N板狀接合體之製造條件 i、主^ 丁 A及各種特性係示於表 衣2 〇 實施例6 係與實施例1同樣在A1N燒結板之立中 1间接/ κf 一面與實施例 门樣形成由TMOJ/zm)以及w(9 以愈每 所構成之金屬層， 貝施例1同樣條件來進行加埶接入 合體。 …接。件到A1N板狀接 示於表 忒Α1Ν板狀接合體之製造條件以及各種特性係 、表 2。 ,、 21 1267498 又，針對此A1N板狀接合體之金屬層的麵曲為19, m/1〇mm’接合界面之剪切強度，包含金屬層之界面為 3.lkgf/mm2’不包含金屬層之界面（燒結板彼此做直接接合 之界面i〇kgf/mm2，再者耐熱經歷特性$ 99%。又，非 接合率Q為〇2%，接人, 接。界面方向之空孔平均長度為3.8// m ’空孔長度比L/Lp之平均為1 ·2。 比較例1 與實施例1完全相同，於其中一面形成金屬層（TiAV)
製作A1N燒結板。 其次，在未形成金屬層之A1N燒結板塗佈做為接著劑 之A1N-Y2〇3漿料（A1N : 1〇〇重量份，乙〇3 : 5重量份，丙 烯酸黏合劑：4重量份，長鏈烴醚系分散劑：〇·5重量份） 之後，豸其疊合於形成有金屬層之前述燒結板（金屬層成為 内側），然後以碳製試樣治具來固定，放入熱壓爐中。
之後，一邊施加負荷300kgf(壓力23 9kg/cm2)一邊在 氮氣氣流中於1650 C保持2小時後，以升溫速度1〇。〔〕/分 麵升酿至1 750 C ’保持4小時。冷卻至室溫後，從爐内取 出’得到以接著劑層做接合之A1N板狀接合體。 所得之A】N板狀接合體，從目視上也可明顯看出翹曲 成碗狀。又，將此A1N板狀接合體表面磨削來平坦化之後 ，所測定之金屬層之翹曲為297 /Zm/1〇mm。又，對於接合 界面之勇切強度進行測定之結果，包含金屬層之界面為 2.〇kg/mm2，不包含金屬層之界面（燒結板彼此做直接接合 之界面）為6kg/mm2，再者耐熱經歷特性為68%。又，非接 22 1267498 JU m 合率Q為2〗.1%，接合界面方向 ，空孔長度比二孔平均長度為ό·5 贲度比L/Lp之平均為4·8。 比較例2 係使用具有应眘& / | /、、知例1相同直押 ，僅改變加熱接合條件(保持溫度、 此以外係以與比較例丨相 '、“間、負荷）’除 。 法來得到A1N板狀接合體 該A1N板狀接合體之 i、表2。 衣&仏件以及各種特性係示於表 比較例3〜9 係使用具有與實施例1相 ，僅改變加熱接合條件（保H技與厚度之趟燒結板 此以外係以與實施例丨相同之皿方;;保持時間、負荷），除 方法來得到A1N板狀接合體 之 製造條件 該A1N板狀接合體 表 以及各種特性係示於表
23 1267498 [表i] 燥部力 齊陰有 輕0 _iR寸 mm 麵 搬 Ra βΙΎΙ 驅 度 μγη 齡 層比 W〇 有無狻 聲 1 齢 纖 1 °c 齡 日· 1 /J诗 ί給 爾 2 °C 齡 綱 2 m 負荷 t 励 kg/cm2 *5删1 0.02 φ4〇Χί6 0.4 1.2 57 Μ j\\\ 1650 2 1750 4 0.3 23.9 窗_2 0.02 φ326Χί30 0.4 1.2 80 Μ j \ \\ 1690 2 1790 4 20 24.0 勣_3 0.02 φ40 X t6 0.4 1.2 57 並 j\ \\ 1650 1 1750 2 0.3 23.9 勣_4 0.02 φ4〇Χΐ6 0.4 1.2 57 ¢2 j\\\ 1650 1 1750 8 0.3 23.9 W_5 0.02 φ4〇Χ t6 0.4 1.2 57 M J\ w 1650 2 1750 4 1 79.6 窗_6 0.02 (j)4〇Xt6 0.4 1.2 57 並 j\\\ 1650 2 1750 4 0.3 23.9 tS鋼1 0.02 φ40 X t6 0.4 1.2 57 有※1 1650 2 1750 4 0.3 23.9 腳1J2 0.02 φ40Χί6 0.4 1.2 57 有※1 1850 6 — — 0.3 23.9 t_U3 0.02 φ40 X t6 0.4 1.2 57 Μ y\\\ 1750 6 — — 0.3 23.9 ttl娜 0.02 φ40 X t6 0.4 1.2 57 無 1800 8 — — 0.3 23.9 腳U5 0.02 ψ40 X t6 0.4 1.2 57 Μ 1600 2 1750 4 0.3 23.9 t_U6 0.02 Φ40Χ16 0.4 1.2 57 j\\\ 1650 0.2 1750 4 0.3 23.9 mwv 0.02 φ4〇Χ 16 0.4 1.2 57 鈿 j\\\ 1650 2 1680 8 0.3 23.9 腳!J8 0.02 φ40 X16 0.4 1.2 57 Μ 1650 2 1750 0.5 0.3 23.9 腳!J9 0.02 φ40 X t6 0.4 1.2 57 Μ j\\\ 1650 2 1750 4 0 0 ※l : ain-y2o3 [表2] 翹曲W ptm 剪切強度 (含金-層) kg/mm2 剪切強g kg/mm2 耐熱經歷 特性 % 非接合率Q % 空孔長度L //111 (平均値） 空孔長度比 L/Lp之平均 實施例1 12 3.8 10.0 100 0.2 1.8 1.1 實施例2 17 3.5 10.0 100 0.2 2.4 1.2 實施例3 13 3.1 10.0 99 0.2 3.4 1.1 實施例4 18 3.2 10.0 99 0.4 1.5 1.4 實施例5 18 3.5 10.0 100 0.3 1.5 1.3 實施例6 19 3.1 10.0 99 0.2 3.8 1.2 比較例1 297 2.0 6.0 68 21.1 6.5 4.8 比較例2 285 1.8 6.8 96 8.5 6.1 5.1 比較例3 250 1.8 5.0 86 12.5 5.2 6.5 比較例4 288 1.8 5.0 75 12.5 5.1 6.5 比較例5 285 2.0 3.0 88 11.5 5.6 8.2 比較例6 244 3.0 6.0 79 11.0 5.6 7.2 比較例7 28 1.5 2.7 89 22.1 5.4 3.1 比較例8 89 2.8 2.5 95 30.0 5.8 3.0 比較例9 350 0.5 0.2 70 52.0 6.2 9.2 24 1267498 【圖式·簡單說明】 ()圖式部分 圖1所示係本發明之A1N板狀接合體之代表性態樣之 部分切開立體圖。 圖2所示係通過圖1中之a 1N板狀接合體中心之側截 面主要部位圖。 圖3係用以說明在A1N板狀接合體所發生之金屬層翹 曲的示意圖。 (二）元件代表符號 氮化鋁燒結體板 氮化鋁燒結體板 金屬層 沿接合界面方向之長度 相對於接合界面在垂直方向之長度 接合體中心 接合界面 線z與金屬層之最大距離 端點間長度 直接接合區域之長度 連、结金屬層端點之線 25

Claims (1)

1267498 拾、申請專利範圍： 1 · 一種氮化鋁接合體，係由··在不使用接著劑之情況 下相互接合之兩片氮化鋁燒結體板、在兩片氮化鋁燒結體 板之接合界面之一部分所形成之金屬層所構成者，其特徵 在於： 一、主 以通過該接合體中心之側截面來觀看時，該接人界面 中之燒結體板彼此直接面對之直接接合區域中係存在著複 數之沿著接合界面之長度L平均為0·5〜4从m之空孔，L 由該空孔形成非接合部， 針對前述側截面，以下述式（1): 非接合率 Q = (X/Y)xl〇〇 ...(1) (式中，X係以在直接接合區域所存在之空孔長度乙之 合計值所表示之非接合部在接合界面方向長度；Y =存在 著空孔之直接接合區域之長度）所算出之非接合率 後在0 · 1〜0 · 5 °/〇之範圍内。 2·如申請專利範圍第1項之氮化鋁接合體，其中，在 該直接接合區域中實質上不存在長度 又l与m以上之空 ，如申請專利範圍第…項之氮化銘接合體，其中 首：空孔沿者接合界面方向之長纟L與對於接合界面在垂 直方向之長度Lp的比（L/Lp)平均為〇.8〜2。 4. 如：請專利嶋丨項之氮化紹接合體，其中，該 孟屬層之遇曲為25// m/i〇nini以下。 5. 如申請專利範圍第1項之氮化叙接合體，其具有 J267498 1〜100mm之厚度。 /·如申請專利範圍帛1項之氮化結接合體，其中，在 歷级=25C到35(TC之升降溫熱經歷達1〇〇次後之該金屬 層與鼠化4呂燒結體板之接合面的剪切強度相對於熱經歷前 之剪切強度為90%以上。 7.一種氮化紹接合體之製造方法，其特徵在於··係由 下述製程所構成者： 準備兩片氮化鋁燒結體板之製程； ”中#氮化銘燒結體板之表面的一部分形成厚度 2 0 // ηι以下之金屬層之製程，· 將2一片氮化铭燒結體板以該金屬層位於中間的方式 4合在前述其中一片氮化1呂燒結體板上形成積層體之製程 ’ 將該積層體一邊以5〜100kg/cm2之壓力加壓一邊以 ㈣⑴峨之溫度進行〇.5〜4小時加熱之製程；以及 其次’使得前述壓力之加壓持續進行，並以超過測 °C且在1 800°C以下之溫度將該積声卿 说领智體加熱2〜8小時之製程 〇 8·如申請專利範圍第7項之靖钆如&人 、<乳化絲接合體之製造方法 ’其中’氮化銘燒結體板之平均表面粗度Ra(m b刪） 位於0·1〜0.8 // m之範圍。 拾壹、圖式： 如次頁。 27
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