200822991 九、發明說明： 【發明所屬之技術領域】 ，本發明係關於包含金屬粒子與揮發性分散媒，且該金屬 粒子之沈降、分離受到抑制的糊狀金屬粒子組成物，以及 使用該糊狀金屬粒子組成物之金屬製構件的黏合方法。 【先前技術】 將銀、銅、鎳等金屬粉末分散於液狀熱硬化性樹脂組成 物中而形成的導電性·熱傳導性糊狀物，係因加熱 化丄形成導電性•熱傳導性被膜。因此，其係被使用於印 刷私路基板上之導電性電路的形成；電阻器或電容器等等 各種電子零件及各種顯示元件之電極的形成；電磁波遮蔽 用導電性被膜之形成；電容器、電阻、二極體、記 =算單元（⑽等晶片零件對基板之黏著；太陽能電'池之 电極的形成’尤其是因為使用非晶石夕半導體而無法進行言 溫處理之太陽能電池之電極的形成；積層陶瓷電容器、： 層陶竞電感器、積層陶莞致動器等晶片型陶变電子、 外部電極的形成等。 v 之 私ίί來’由於晶片零件之高性能化，來自於晶片零件之 ★…、里增加’除了原本要求之電傳導性以外，亦要求 :性之提升。因此，藉由儘可能地增加金屬粒子之含有 率，期望提升電傳導性、熱傳導性。然而有 則=之黏度會上升，而有作業性顯著降低之 為了解决此種問題，本案發明人等發 與揮發性分散媒所構成之糊狀銀組成物μ加熱， 312ΧΡ/發明說明書(補件)/96-07/96109691 , 〇 200822991 發性分散媒會揮發，銀粉末進行燒結，可形成具有極高導 電性與熱傳導性之固狀銀，並發現其對於金屬製構件之黏 合或導電電路之形成非常有用，因而提出專利申請（曰本 專利特願2005-152827、特願2005-309126)。但是，本案 發明人等亦發現，由銀、銅、鎳之類的比重較大之金屬粒 子與比重較小之揮發性分散媒所構成之糊狀組成物，由於 兩者之比重差大，因此具有金屬粒子會經時性分離並沈降 之問題。 一於日本專利特開2005一93380中，提案有由銀粉末與多 元醇類所構成之銀油墨，以及由銀粉末、多元醇類與黏度 調整劑（水、酮類或醇類）所構成之銀油墨。另外記載"了二 藉由併用多元醇類與酮類或醇類，可提升分散性。然而， 本發明人等發現，如銀、銅、鎳之類的比重較大之金屬粒 子與比重較小的多兀醇類以及黏度調整劑所構成之糊狀 組成物，由於兩者的比重差大，因此具有金屬粒子會經時 性分離並沈降之問題。 (專利文獻1)日本專利特開2005-93380 【發明内容】 (發明所欲解決之問題） 本發明人等深入研究不具上述問題之糊狀金屬粒子組 成物，亦即，金屬粒子與揮發性分散媒之經時性分離受到 抑制’且比重大的金屬粒子之沈降亦受到抑制之糊狀金屬 粒子組成物。結果發現，藉由選擇金屬粒子表面之被覆劑 與揮發性分散媒，可抑制糊狀金屬粒子組成物中金屬粒子 312XP/發明說明書(補件)/96-07/96109691 η 200822991 之分離、沈降，因而完成本發明。本發明之目的在於提供 即使經過長期間保存，仍可抑制比重大的金屬粒子自揮發 性分散媒分離、並抑制金屬粒子沈降，亦即保存安定性優 •異之糊狀金屬粒子組成物，並提供使用該糊狀金屬粒子組 -成物而牢固黏合金屬製構件之方法。 (解決問題之手段） 上述目的可藉由下述發明達成： 0 [丨]一種糊狀金屬粒子組成物，其特徵為包含：（A)100 重量份之金屬粒子，其係平均粒徑〇· 〇〇丨〜“# m，表面被 撥水性有機物被覆；以及（B)3〜30重量份之揮發性分散 媒；該揮發性分散媒（B)係包含介電係數不同之揮發性分 散媒（B1)與揮發性分散媒（B2)，且揮發性分散媒（B1)與揮 毛性为政媒（B 2 )係為常溫下不完全相溶之混合比率。 [2] 如[1]之糊狀金屬粒子組成物，其中，撥水性有機物 係為咼級脂肪酸、高級脂肪酸醯胺或高級脂肪酸酯，金屬 、粒子（A)之金屬係為金、銀、銅、把、鎳、錫、銘或該等 之合金。 [3] 如[2]之糊狀金屬粒子組成物，其中，金屬粒子（A) 係被高級脂肪酸被覆之銀粒子。 、 [4]如[1]之糊狀金屬粒子組成物，其中，揮發性分散媒 -(B1)與揮發性分散媒（B2)係選擇自下列群組：水、揮發性 1元醇、具醚鍵結之揮發性1元醇、揮發性多元醇、揮發 性烴、揮發性醚、揮發性脂肪酸酯、揮發性酮、揮發性脂 肪l S篮胺、揮發性脂肪族胺以及烧基猜；且，該揮發性分 312XP/發明說明書(補件)/96-07/96109691 8 200822991 散媒（B1)與該揮發性分散媒（82)於25Ct之介電係數的差 在2. 0以上。 [5 ]如[1 ]之糊狀金屬粒子組成物，其中，揮發性分散媒 (β1)與揮發性分散媒（B2)之混合比率為98 ·· 2〜2 ·· 98。 [6 ]如[4 ]之糊狀金屬粒子組成物，其中，揮發性分散媒 (Β1)與揮發性分散媒（β2)之混合比率為98 ·· 2〜2 ·· 98。 [7 ] —種金屬製構件之黏合方法，其特徵為，使[1 ]〜[6 ] 中任一項之糊狀金屬粒子組成物介隔存在於多個金屬製 構件間，藉由加熱、藉由一邊加壓並施加超音波振動、或 者藉由加壓及加熱並施加超音波振動，使揮發性分散媒揮 散，將金屬粒子（Α)彼此進行燒結，藉此使多個金屬製構 件彼此黏合。 [8]—種糊狀金屬粒子組成物，其特徵為包含：（Α)1〇〇 重量份之金屬粒子，其係平均粒徑〇· 001〜50// ra，表面被 撥水性有機物被覆；以及（C)3〜30重量份之揮發性分散 媒，其係25°C之介電係數為30〜75，不拒斥金屬粒子（A)。 [9 ]如[8 ]之糊狀金屬粒子組成物，其中，撥水性有機物 係為南級脂肪酸、高級脂肪酸醯胺或高級脂肪酸酯，金屬 粒子（A)之金屬係為金、銀、銅、把、錄、錫、銘或該等 之合金。 [10]如[9]之糊狀金屬粒子組成物，其中，金屬粒子（a) 係被高級脂肪酸被覆之銀粒子。 [11 ]如[8 ]之糊狀金屬粒子組成物，其中，揮發性分散 媒（C)為揮發性多元醇、二曱基曱醯胺或揮發性1元醇水 312XP/發明說明書(補件)/96-07/96109691 9 200822991 溶液。 [12]—種金屬製構件之黏合方法，其特徵為，使[7]〜u川 中任一項之糊狀金屬粒子組成物介隔存在於多個 構件間，藉由域、藉由-邊加壓並施加超音波振動、或: 者猎由加壓及加熱並施加超音波振動，使揮發性分散媒⑹ 揮散，將金屬粒子（A)彼此進行燒結，藉此使多個金屬製 構件彼此黏合。 (發明效果） 本赉明之糊狀金屬粒子組成物即使經長期間保存，仍可 ，制比重大的金屬粒子與比重小的揮發性分散媒（8)分 離，並抑制比重大的金屬粒子（A)a生沈降，可保持均勻 的糊狀物狀態。 根據本發明之黏合方法，金屬製構件間之糊狀金屬粒子 組成物係藉由加熱而使該揮發性分散媒揮散，經由在該金 屬粒子（A)之燒結溫度以上的溫度下加熱，該金屬粒子（a) 彼此燒結而成為固體狀，可牢固地黏合多個金屬製構件彼 此。 【實施方式】 本發明之糊狀金屬粒子組成物之特徵在於，係包含·· (A)100重量份之金屬粒子，其平均粒徑為〇〇〇1〜5〇#m， 表面係被撥水性有機物被覆；以及（B)3〜3〇重量份之揮發 性为政媒，该揮發性分散媒（B )係含有介電係數不同之揮 餐性为政媒（B1)與揮發性分散媒（B2 ),且揮發性分散媒（b 1) 與揮發性分散媒（B2)係於常溫下不完全相溶之混合比率。 312XP/發明說明書(補件)/96-07/96109691 10 200822991 、/屬粒子（A)之表面必須被撥水性有機物所被覆。該有 機物最好為潤滑性亦佳，以高級脂肪酸、高級脂肪酸金屬 孤（仁鹼^屬鹽除外）、高級脂肪酸醯胺及高級脂肪酸酯為 尤以同級脂肪酸特佳。撥水性有機物之被覆量係因金 屬粒子之粒徑、比表面積、形狀等而異，較佳為金屬粒子 之0·01〜3重，更佳為〇·2〜2重量％。若過少則保存 安定性下降，若過多則加熱燒結性下降。 屬粒子（Α)之材質係常溫下為® Μ，只要可經加孰或 加熱與施加超音波振動而燒結即可，可例示金、銀、銅戈 錫、紹以及該等之合金。該等之中，以銀、銅、 自加熱燒結性、熱傳導性及導電性之觀點而言， 二厘么銀粒子可僅其表面—部份或全部均為氧化銀。 子（Α)之平均粒徑為〇〇〇1〜5〇^。該平均粒徑 /、用田射繞射散射式粒度分佈敎法所得之 屬It若平均粒徑超過5〇⑽則變得難以防止金 ==因此，平均粒徑較小者為佳，以2一以 面、^=而Γ胃奈米尺寸之未滿0々m之情況，表 之虡。因此’以。存安定性降低 屬粒子⑴之形狀為球狀、大致球狀°.》更佳。金 M ^ , 大致球狀大致立方體狀、碎 較佳為碎片狀則形狀等。自保存安定性之觀點而言， 尤佳者為將還原法製作之銀粒子予 雖提案有多種利㈣原法之絲子的製造方法，但一 ^係 312XP/發明說明書(補件)脉_61〇9691 Μ 200822991 ^肖酸銀讀液中加人氫氧_水溶液，製作氧化銀，將 八加入褐馬林之類的還原劑之水溶液中，藉此還原氧化銀 而生成銀粒子，再進行水洗、過濾、乾燥等。 .撥水性有機物所附著之碎片狀金屬粒子，可對例如球狀 •之粒狀金屬粒子添加撥水性有機物，以球磨等進行粉碎， 便可衣造（參照日本專利特公昭4〇_6971、特開 2000-2341 07 之[〇〇〇4])。 r -將粒狀金屬粒子與高級脂肪酸、高級脂肪酸金屬鹽（但 鹼至屬鹽除外）、兩級脂肪酸酯、高級脂肪酸醯胺等撥水 性有機物，與陶兗製之球一起投入旋轉式鼓裝置（例如球 磨）中，以球物理性地拍打金屬粒子，藉此可容易地加工 成碎片狀（鱗片狀）。此時，用以提升潤滑性之高級脂肪 酸、高級脂肪酸金屬鹽（但鹼金屬鹽除外）、高級脂肪酸 酯、高級脂肪酸醯胺等撥水性有機物，係附著於碎片狀金 屬粒子上。作為此種高級脂肪酸，可例示月桂酸、肉豆蔻 (k、棕櫚酸、硬脂酸、油酸、亞麻油酸、次亞麻油酸，較 佳為高級飽和脂肪酸。作為此種高級飽和脂肪酸，可例示 月桂酸、肉豆蔻酸、棕櫚酸、硬脂酸。碎片狀金屬表面只 要以此種高級脂肪酸等被覆一半以上即可，但以全部被覆 - 為佳。此種金屬表面被撥水性有機物被覆之金屬粒子，係 • 顯示撥水性。若撥水性有機物之附著量過少，則金屬粒子 變得容易分離沈降，若過多則燒結性降低。因此，撥水性 有機物之附著量較佳為〇· 01〜3%，更佳為〇. 1〜1 %。撥水 性有機物之附著量可以一般方法測定。例如可例示：在氮 312沿/發明說明書(補件)/96-07/96109691 12 200822991 氣十加熱至撥水性有機物之沸點以上，測定重量減少之方 法’將金屬粒子在氧氣氣流中加熱，將附著於金屬粒子之 抵水性有機物中的碳轉變為二氧化碳，並利用紅外線吸收 光譜法進行定量分析之方法。 將表面以撥水性有機物被覆之金屬粒子（A)亦可利用一 般方法製造。例如可藉由將金屬粒子浸潰於撥水性有機物 之/谷液中’取出金屬粒子並乾燥而製造。 揮發性分散媒（B)係由介電係數不同之揮發性分散媒 (B1)與揮發性分散媒（B2)所構成，並且， ^ 與揮發性分散媒⑽係於常溫下不完全相溶之ντζ 合物。 是否不完全相溶，可利用下述方法判定。 亦即，於玻璃容器内攪拌混合揮發性分散媒（Bl)盘 ^生分，媒⑽，靜置至氣泡消失後，以目視觀察。當分離 為者呈混濁之情況’可判定為不相溶。當 一層且透明，可判定為相溶。 n :揮發性分散媒⑽與揮發性分散媒⑽相溶而成為 離勾之狀：’則糊狀金屬組成物中之金屬離子( =生因^法防止沈降現象。關於揮發性分散 媒⑽之混合比率’只要不完全相溶即可 率較佳為在99 : 2〜2 : 99之範圍内。 及比 為了將本發明之糊狀金屬粒子組成物^ k結性或加熱·超音波振動燒結性之 *二，、口”、、 散媒不為非揮發性，必須為揮發性/二、4著劑’分 凡具在金屬粒子（A) 312XP/發明說明書(補件)/96-07/96109691 13 200822991 為銀粒子之情況，若彡 易燒結，容易利用作^=放媒揮散，則銀粒子變得容 揮發性分㈣之沸1 5劑、黏著劑’因此有上述限制。 若沸點未滿6(TC，二6〇C〜3〇〇C為佳。其原因在於， 物之作業中揮散若=1容易在㈣糊狀金屬粒子組成 性分散媒⑻仍會殘留。‘.於300 c ’則即便加熱後揮發 此種揮發性分散媒（β)可選 所構成之揮發性煙化合物；由原，、及氫原子 構成之揮發性有機化合物;由碳々：、=:二氧原子所 構成之揮發性有機化合物；由碳原子、及，原子所 氮原子所構成之揮發性有機物&氧原子及 液狀。 …生有枝化合物荨。該 等在常溫下均為 具體而言可例千· 士 · 庚醇、奈旷水，乙鮮、丙醇、丁醇、戊醇、己醇、 附田甘醇、癸醇等揮發性一元醇；乙二醇單甲A ，基賽路蘇、甲基卡必醇)、乙二醇單乙基二= 基卡必醇h乙二醇單丙基_ (丙基赛路蘇、丙基 h乙二醇單丁絲（丁基赛珞蘇、丁基卡必醇）、 一:醇单甲基_、甲基甲氧基丁醇等具有賴結之揮發性 节醇、2-苯基乙基醇等揮發性芳烷基醇；乙二醇、 丙一醇、甘油等揮發性多元脂肪族醇；低級正石蠟、低級 ^石壤等揮發性脂肪族烴；曱苯、二甲苯等揮發性芳香族 二’丙酮、曱基乙基酮、曱基異丁基酮、環己酮、二丙酮 • (4~羥基一4—曱基一2一戊酮）、2-辛酮、異佛酮（3,5,5一三 曱基—2-環己烯一一酮）、二異丁基酮（2,6_二曱基_4—庚綱^ 312ΧΡ/發明說明書(補件)/96-07/96109691 14 200822991 等揮發性脂肪族酮；醋酸乙酯（乙基醋酸酯）、醋酸丁酯、 乙醯氧基乙烷、丁酸曱酯、己酸曱酯、辛酸曱酯、癸酸曱 酯、曱基赛珞蘇醋酸酯、丙二醇單曱基醚醋酸酯等之揮發 性脂肪族羧酸酯；四氳ϋ夫Π南、二丙基_、乙二醇二曱基鍵、 乙二醇二乙基醚、乙二醇二丁基醚、丁二醇二曱基醚、乙 氧基乙基醚等揮發性脂肪族醚；低分子量之揮發性矽酮油 及揮發性有機改質矽酮油；乙醯胺、Ν，Ν一二曱基曱醯胺等 之揮發性羧酸醯胺；曱基胺、乙基胺、丙基胺、伸乙二胺 等之揮發性1級脂肪族胺；二甲基胺、二乙基胺等之揮發 性2級脂肪族胺；三曱基胺、三乙基胺等之揮發性3級脂 肪族胺；其他揮發性脂肪族胺；乙腈、丙腈等揮發性烷基 腈。水以純水為佳，其電傳導度較佳為l〇〇/zS/cm以下， 更佳為10 // S/cra以下。純水之製造方法以一般方法即 可’可例示離子交換法、逆滲透法、蒸鶴法。 揮發性分散媒（B1)與揮發性分散媒（B2)必須從上述揮 ，發性分散媒（B)選擇25°C下之介電係數差為2以上者，較 佳為3以上，更佳為選擇5以上者。 作為揮發性分散媒（B1)，較佳係選擇25°C下之介電係 數面的水、揮發性1元醇、揮發性多元醇、揮發性芳烧笑 •醇、N，N-二曱基曱醯胺、揮發性脂肪族胺、揮發性脂肪族 _、揮發性脂肪族羧酸酯或揮發性脂肪族酮，作為揮發性 分散媒（B2)，較佳係選擇25°C下之介電係數較揮發性分 政媒（B1)小2以上（較佳為小3以上，更佳為小5以上） 之揮發性脂肪族醚、揮發性脂肪族羧酸酯、揮發性脂肪族 312XP/發明說明書(補件)/96-07/96109691 15 200822991 酮、士揮發性脂肪族烴、揮發性芳香族烴或揮發性㈣油。 此日广，揮發性分散媒⑻）與揮發性分散媒⑽）於 25〇C 下 之”電係數之差若為2以上（較佳為3以上，更佳為5以 上）’則亦可為同種之有機化合物。 ^揮卷性刀放媒（β〗）與揮發性分散媒（B2)於Μ。。之介電 ί數的f絲滿2，則兩揮發性分散媒彼此的相溶性變 问不谷易防止糊狀金屬粒子組成物中金屬粒子（A)之分 離、沈降。 25 C下之介電係數之差為2以上（較佳為3以上，更佳 為5以上），雖所選擇之揮發性分散媒（Μ)與揮發性分散 媒（B2)仍會某程度地相溶，但必須不完全相溶。又，與金 屬粒子（A)調配時，揮發性分散媒（B1)與揮發性分散媒'(B2) 雖某程度地相溶，但必須為不完全相溶的混合比率。 另外，亦可將揮發性分散媒（B1)、（B2) 一起併用2種以 上，但必須為（B1)與（B2)混合時不相溶之混合比率。 揮發性分散媒（B)之調配量、亦即揮發性分散媒（B1)鱼 揮發性分散媒（B2)之合計調配量，每1〇〇重量份之金屬粒 子（A)為3〜30重量份，此係在常溫中使金屬粒子（A)成為 糊狀之充足量。本發明之糊狀金屬粒子組成物中，只要不 悖離本發明之目的，亦可少量或微量含有金屬粒子（A)以 外之非金屬系粉體、金屬化合物、金屬錯合物、搖變劑、 安定劑、著色劑等之添加物。 Μ 本舍明之糊狀金屬粒子組成物可藉由將下述成分置入 混合器中，攪拌混合至呈現均勻為止而容易地^造： 312ΧΡ/發明說明書(補件)/96-07/96109691 16 200822991 (A)100重量份之金屬粒子，其係平均粒徑〇 〇〇1~5〇//m， 表面被撥水性有機物被覆；以及（B)3〜3〇重量份之揮發性 刀放媒。揮發性分散媒（βΐ)與揮發性分散媒（β2)可預先混 合而有某種程度的相溶性，亦可以不完全相溶的狀態與金 屬粒子（Α)混合。或者，亦可分別混合揮發性分散媒（β1) 與揮發性分散媒（Β2)。 本發明之糊狀金屬粒子組成物係金屬粒子（八彡與揮發性 分散媒⑻之混合物，常溫下為糊狀。另夕卜，糊狀係包含 霜（cream)狀。藉由糊狀化，可從注射器或喷嘴吐出為細 線狀，又，利用金屬遮罩容易進行印刷塗佈。 本發明之其他實施態樣的糊狀金屬粒子組成物之特徵 為含有（A)100重量份之金屬粒子，其係平均粒徑 〇. 001〜5〇e m，表面被撥水性有機物被覆；以及 重量份之揮發性分散媒，其係25乞之介電係數為3〇〜M 者。由於金屬粒子（Α)被撥水性有機物被覆，因此，藉由 與介電係數30〜75之揮發性分散媒併用，可抑制分離•沈 降。若金屬粒子未被撥水性有機物被覆，即便與揮發性^ 散媒（C)併用，仍無法抑制分離·沈降。 金屬粒子（A)係如上所述。 揮發性分散媒（C)可由下述之中選擇25°c之介電係數為 30〜75者：由碳原子、氫原子及氧原子構成之揮發性機 化合物；由碳原子、氫原子及氮原子構成之揮發性有播 合物；由碳原子、氫原子、氧原子及氮原子構成之揮發性 有機化合物等。具體而言，可自25t：之介電係數為 312ΧΡ/發明說明書(補件)/96_〇7/96ΐ〇9691 17 200822991 之揮發性一元醇、揮發性多元醇、揮發性低級脂肪族羧酸 醯胺、揮發性烷基腈及揮發性醇（例如揮發性一元醇、揮 發性多元醇）之水溶液選擇。 作為此種揮發性分散媒，可例示甲醇等揮發性一元 低級醇；揮發性一元低級醇（例如乙醇）之水溶液，·乙二 醇、丙二醇、甘油等揮發性多元醇；乙醯胺、二甲基甲醯 胺等揮發性低級脂肪族羧酸醯胺、乙腈、丙腈等揮發性烷 基腈。該等之中，以介電係數3〇〜7〇之多元醇為佳。另外， 併用2種以上之分散媒時，該混合物於託它之介電係數 為30〜75即可。 揮發性分散媒（C)的調配量係每重量份之金屬粒子 (A)為3 3 0重里伤，為將金屬粒子（a )糊狀化所需之充分 畺本杳明之上述糊狀金屬粒子組成物，只要不悻離本發 明之目的，亦可少量或微量含有金屬粒子以外之非金屬系 知體、金屬化合物、金屬錯合物、搖變劑、安定劑、著色 劑等之添加物。 本發明之上述糊狀金屬粒子組成物可藉由將下述成分 置入混合器中，攪拌混合至呈現均勻為止而容易地製造： (A)l〇〇重量份之金屬粒子，其係平均粒徑〇· 〇〇1〜5〇#❿， 表面被撥水性有機物被覆；以及（c) 3〜3〇重量份之揮發性 分散媒。 本發明之上述糊狀金屬粒子組成物係金屬粒子（A)與揮 發性分散媒（C)之混合物，於常溫下為糊狀。另外，糊狀 亦包含霜狀。藉由糊狀化，可從注射器或喷嘴吐出為細線 312XP/發明說明書(補件)/96-07/96109691 18 200822991 狀，又，可容易利用金屬遮罩進行印刷塗佈。 本1明之上述2種糊狀金屬粒子組成物係經由加埶 揮發性分散媒揮發。本發明之上述2種糊狀金屬粒子:成 物中藉由加熱至金屬粒子的燒結溫度以上之溫度，戋者 藉由一邊加壓並施加超音波振動，尤其是一邊加壓、加熱 亚施加超音波振動，使揮發性分散媒（B)或揮發性分散媒、 (C)揮散，該金屬粒子（A)彼此燒結，成為強度、導電性與 熱傳導性優異之固形狀金屬。亦可於糊狀金屬粒子組成物 之加熱時施加壓力。此時，可使揮發性分散媒⑻或揮發 性分散媒⑹揮散’接著燒結金屬粒子（a)彼此，亦可使揮 發性分散媒⑻或揮發性分㈣⑹揮散，㈣燒結金屬粒 子（A)彼此。尤其在金屬粒子（A)為銀粒子之情況，由於銀 原本便具有高強度與極高電傳導性及熱傳導性，因此，本 毛月之銀粒子彼此的燒結物亦具冑高強度與極高電傳導 性及熱傳導性。此時之加熱溫度只要為使揮發性分散媒⑻ 或揮毛生刀政媒（C)揮散而銀粒子可燒結之溫度即可，通 常為loot以上，尤以15(TC以上為佳。然而，若超過4〇〇 °C，則揮發性分散媒會以突彿方式蒸發，可能對固形狀金 屬之形狀造成不良影響，因此必須在4〇(rc以下，較佳為 300°C以下。僅利用加熱不易燒結之金屬粒子（A)，亦藉由 一邊加壓並施加超音波振動，或者一邊加壓、加熱並施加 超音波振動，而可良好地燒結。 超音波振動之頻率為2kHz以上，i〇kHz以上為佳。其 上限並無特別限制，以裝置能力而言大約為5〇〇kHz。又， 312XP/發明說明書(補件)/96-07/96109691 19 200822991 超:波振動之振幅會影響燒結性，因此較佳為0. 1〜40//m， 更仏為0.3 20//m，尤佳為〇·5〜。另外，為了使超 音波振動確實傳達至糊狀金屬粒子組成物，較佳係將超音 波振動之發射部分直接抵接於 糊狀金屬粒子組成物。或 者透過不易吸收超音波振動之素材所構成之覆蓋材等， 將超音波振動之發射部分抵接。對糊狀金屬粒子組成物之 抵接疋力’較佳為〇· 9kPa(0. 09gf/mm2)以上，更佳為 9kPa(j· 92gf/_2)以上，尤佳為 39kpa(3· 98gf/_2)以上， 抵接壓力之上限為不破壞黏合之構件的壓力之最大值。 一邊加壓、加熱並施加超音波振動而燒結的情況之加熱 溫度，只要較常溫高，且為揮發性分散媒（B)或揮發性分 散媒（C)可揮散而金屬粒子可燒結之溫度即可。然而， 若加熱溫度超過400°C，則揮發性分散媒（B)或揮發性分 散媒（C)會以突沸方式蒸發，可能對固形狀金屬之形狀造 成不良影響，因此以400t以下、且未滿該金屬粒子（A) 之溶點的溫度為佳，較佳為3 〇 〇 以下。 該金屬粒子（A)燒結而成之固形狀金屬的形狀並無特別 限制，可例示薄片（sheet)狀、薄膜狀、帶狀、線狀、圓 盤狀、塊狀、點狀、不規則形狀。 本發明之上述2種糊狀金屬粒子組成物係藉由加熱，或 者藉由一邊加壓並施加超音波振動，或者是一邊加壓、加 熱並施加超音波振動，使揮發性分散媒（β)或揮發性分散 媒（C)揮散，金屬粒子燒結。燒結而成之固形狀金屬係強 度與電傳導性、熱傳導性優異，具有對於接觸之金屬製構 312ΧΡ/發明說明書(補件)/96-07/961〇9691 20 200822991 : : := 基板、鍍銀金屬基板、銅基板、銘 鎳基板、鍍錫金屬基板等金屬系基 =絕緣性基板上之電極等金屬部分的黏著性，因此， 基板或具有金屬部分的電子零件、電子裝置、電 :冬件、電氣裝置等之黏合方面有用。此種黏合可例示電 奋益、電阻等日日日片零件與電路基板之黏合；二 體义、咖等半導體晶片與引線框架或電路基板之黏合； 叙熱之CPU晶片與冷卻板之黏合。 將本發明之上述2種糊狀金屬粒子組成物燒結以後，由 於不殘存刀政媒’因此不需洗淨，但亦可以水或有 洗淨。 由於本發明之上述2種糊狀金屬粒子組成物含有揮發 =散媒⑻或揮發性分散媒⑹，因此較佳係保存於密閉 谷益中。亦可為了提升保存安定性而進行冷藏保管，保管 溫度可例示1 〇 °c以下。 [實施例] 以下揭示本發明之實施例與比較例。實施例與比較例 中，記載為「份」者係表示「重量份」。金屬粒子中之撥 水性有機物量的測定方法、揮發性分散媒之介電係數的測 疋方法、糊狀金屬粒子組成物保管中之金屬粒子與揮發性 分散媒之分離性的測定方法、以及藉由將糊狀金屬粒子組 成物加熱或進行超音波熱壓合而燒結所生成之固形狀金 屬的黏著強度’係利用下述方法測定。另外，未特別記載 之情況的溫度為25°c。 312XP/發明說明書(補件)/96-〇7/96109691 200822991 [撥水性有機物量] 利用πίΑ法如下述般進行測定。將金屬粒子於氮氣氣流 中以io:c/:鐘之速率升溫至5〇rc，直接在5〇(rc下保 持1小時。定義[加熱前重量—加熱後重量]/[加熱前重量] xl〇〇 =撥水性有機物量（單位％)。 [介電係數] 利用液體介電係數測定裝置（Scientific^公司製，型 號870)進行測定。 < [金屬粒子與揮發性分散媒之分離性] 將糊狀金屬粒子組成物！置入安裝有前端蓋2之注射器 3(内徑12mm，長度55mm，内容積5cc，EFD公司製），使 注射器3之前端部朝下至3〇mm之高度為止，安裝活塞4， 最後安裝尾端蓋5而密閉。將注射器3之前端部朝下並垂 直保持，靜置24小時。測定注射器3内之糊狀金屬粒子 組成物1中，分離至上部的揮發性分散媒層之厚度（mm)。 [黏著強度A ] 使用iOOp厚之金屬遮罩，對寬度25mmx長度75麵 厚度Ιππη之鍍銀銅板塗佈糊狀金屬粒子組成物（塗佈面 積：5imnX5inm)，於其上搭載寬度5mmx長度5mmx厚度〇 5咖 之銀製晶片後，於強制循環式烘箱内以2〇(rc加熱丨小 時，藉此使銀製晶片黏著於鍍銀銅板。將如此製得之黏著 強度測定用試驗體安裝於模頭剪力（Die讣的/)強度^定 試驗機，以模頭剪力強度測定試驗機之模頭剪力工具，以 23mm/分鐘之速度按壓銀製晶片之側面。 以銀製晶片與鍍 312XP/發明說明書(補件)/96-07/96109691 22 200822991 銀銅板間之黏合部被剪切破壞時之負重為黏接強度（單 位：kgf)。另外，黏著強度試驗係進行3次，以其平均值 為黏著強度A。 - [黏著強度B ] 使用100/zm厚之金屬遮罩，對寬度25腿χ長度75mmx 厚度1mm之鍍銀銅板塗佈糊狀金屬粒子組成物（塗佈面 積：Smmdnnn)，於其上搭載寬度5mmx長度5_χ厚度〇. 5咖 之銀製晶片，製作接著強度測定用前體。將黏著強度測定 用前體安裝於超音波熱壓黏裝置，以超音波振動之頻率 30kHz、超音波振動之振幅4em、抵接壓力1〇〇N/cm2之條 件，將超音波熱壓黏裝置之壓黏部（探針）自上方抵接於該 黏著強度測定用前體之銀製晶片的上部，一邊施加超音波 振動，一邊以20(TC之溫度壓黏3〇秒。將如此製得之黏 著強度敎用試驗體安裝於模頭剪力強度測^試驗機，以 模頭剪力強度測定試驗機之模頭剪力丄具，以23mjn/分鐘 之速度按壓銀製晶片之側面。以銀製晶片與鑛銀銅板間之 黏合部被剪切破壞時之負重為黏接強度(單位：以。。另 外，黏著強度試驗係進行3次，以其平均值為黏 [實施例1] 將市售之以還原法製造的銀粒子碎片化，製作i次粒子 :粒徑為3. 〇 A m(以雷射繞射法測定)之碎片狀銀粒 水性ini5重量％之硬脂酸被覆，該銀粒子具有撥 、》之上述碎片狀銀粒子添加12份之苄醇（和 先,、，屯樂工業股份有限公司販售之試藥，介電係數13.(〇作 312XP/發明說明書(補件)/96-07/96109691 23 200822991 為揮發性分散媒（B1)及3份之1-己烷（和光純藥工業股份 有限公司販售之試藥，介電係數2·〇)作為揮發性分散媒 (B2)，使用漿葉攪拌器均勻混合，藉此調製糊狀銀粒子組 成物。作為揮發性分散媒（B1)之苄醇12份與作為揮發性 刀放媒（B2)之1 -己烧3份的混合物，係不相溶的比率。 將兩者攪拌、混合便產生白濁現象，予以靜置便馬上分離 為2層。 该糊狀銀粒子組成物於注射器内並未觀察到銀粒子與 揮發性分散媒之分離。測定該糊狀銀粒子組成物之黏著強 度’結果係整合示於表i。由以上結果可知，該糊狀銀粒 子組成物並無銀粒子與揮發性分散媒之分離，保存安定性 優異，於強力黏合金屬製構件方面係有用的。 [實施例2] 於實施例丨中’除了取代銀粒子，使歸料之銅粒子 碎片化而製作i次粒子的平均粒徑為Up(以雷射繞射 if疋）之碎片狀銅粒子（銅表面被G.5重量％之硬脂酸 =覆’該銅粒子具有撥水性）以外，與實施例i同樣地調 ^胡狀銅粒子組成物。該糊狀銅粒子組成物於注射器内並 t觀察到銅粒子與揮發性分散媒之分離。結果係整合示於 由以上結果可知， 發性分散媒之分離， [實施例3] 該糊狀銅粒子組成物並無銅粒子與揮 長日守間之保存安定性優異。 將市售之鎳粒子碎片化 製作1次粒子的平均粒徑為 312XP/發明說明書(補件)/96-07/96109691 200822991 6.°=雷射繞射法測定)之碎片狀 狀鎳粒子添加12份之N N—_ w A w (和光純藥卫業股份有限公司販f之’甲醢胺 及3份之卜己 : = = :性:散媒⑽之卜己炫3份的混合物，係 置便馬上分離為2層。便產生白濁現象’予以靜 揮：:，粒子組成物於注射器内並未觀察到錄粒子與 :刀放媒之分離。結果係整合示於表卜由以上 ==糊士狀錄粒子組成物並無錄粒子與揮發性分散叙 刀離長蚪間之保存安定性優異。 [實施例4] 將市售之以還原法製造的銀粒子碎片化，製作丨次粒子 :平均粒徑為3.0/^(以雷射繞射法測定)之碎片狀銀粒 銀表面被0·5重量％之硬脂酸被覆，該銀粒子具有撥 水性），對100份之上述碎片狀銀粒子添加u份之雙（2一 =氧基乙基）醚（和光純藥工業股份有限公司販售之試 藥，介電係數5.6)作為揮發性分散媒（B1)& 4份之乙二 醇（和光純藥工業股份有限公司販售之試藥，介電係數 39.〇)作為揮發性分散媒（B2)，使用漿葉攪拌器均勻混 312XP/發明說明書(補件)/96-07/96109691 25 200822991 乙14 土 土㈣11份與作為揮發性分散媒（B2)之 乙一醇4伤的混合物，得又士々 # ^ ^ , ^ Ιθ .工’、相浴的比率。將兩者攪拌混合 便產生白濁現象，予以靜置便馬上分離為2層。 该糊狀銀粒子組成物於沐身 +哭、 ^ 取物於，主射态内亚未觀察到銀粒子與 揮舍性分散媒之分離。測定兮也 〆 、疋孩糊狀銀粒子組成物之黏著強 度’結果係整合示於表1。由 由以上、、、口果可知，該糊狀銀粒 子組成物並無銀粒子與揮發性分㈣之分離，保存安定性 優異，於強力黏合金屬製構件方面係有用的。 [實施例5] 對_份之市售之以沈殿法製造、μ粒子的平均粒徑 為1· 1//ιη(以雷射繞射法測定）之粒狀銀粒子（銀表面被 1.5重量％之硬脂酸被覆，該銀粒子具有撥水性），添加 14份之1,2-二乙醯氧基乙烷（和光純藥工業股份有限公 司販售之試藥’介電係數7. 3)作為揮發性分散媒（βι)及2 ，之Isozol 300(新日本石油股份有限公司販售之異石蠟 混合物，介電係數2. 1)作為揮發性分散媒（β2)，使用漿 葉攪拌器均勻混合，藉此調製糊狀銀粒子組成物。作為揮 發性分散媒（Β1)之1,2-二乙醯氧基乙烷14份與作為揮發 性分散媒（Β2)之Is〇z〇i 300 2份的混合物，係不相溶= 比率。將兩者攪拌混合便產生白濁現象，予以靜置便馬上 分離為2層。 、 該糊狀銀粒子組成物於注射器内並未觀察到銀粒子與 揮發性分散媒之分離。測定該糊狀銀粒子組成物之黏著強 312XP/發明說明書(補件)/96-07/96109691 26 200822991 度，結果係整合示於表1^由以上結果可知，該糊狀銀粒 子組成物並無銀粒子與揮發性分散媒之分離，保存安定性 優異，於強力黏合金屬製構件方面係有用的。 [實施例6] 於貝施例5中，除了作為揮發性分散媒（β1)係取代丨，2一 二乙醯氧基乙烧而使用甲基正己基_ (和光純藥工業股份 有限公司販售之試藥’介電係數12.2)14份，並取代揮發 性分散媒（B2)而使用純水（蒸鶴水，介電係數8〇〇)2份以 外，與實施例5同樣地調製糊狀銀粒子組成物。作為揮發 =散媒⑽之甲基正己基_14份與作為揮發性分散媒 (B2)之純水2份的混合物，係不相溶的 混合便產生白濁現象。 言稅择 該糊狀銀粒子組成物於注射器内並未觀察到銀粒子盥 =發性分«之分離。敎該糊狀銀粒子組成物之黏著強 度，結果係整合示於表1。由以上 不h M上結果可知，該糊狀銀粒 ^成物並無絲子與揮發性分散叙分離，健安定性 釔異，於強力黏合金屬製構件方面係有 [實施例7] 將市售之以還原法製造的銀粒子碎片化，製作卜 的平均粒徑為3.0/zm(以雷射繞 ，子 子歸面被0.5重量％之硬脂之碎片狀銀粒 水性)，對丨。。份之上述碎片二被子:加^ (和光純藥工業股份有限公司販售之試藥加八 15,之乙二醇 作為揮發性分散媒（c)吏 :；|電係數39. 0) 使用疑轉式混練機均勻混合，藉 312XP/發明說明書(補件)/96-07/96109691 27 200822991 此调製糊狀銀粒子組成物。 八：：^銀：子組成物於注射器内並未觀察到銀粒子與 二定該糊狀銀粒子組成物之黏著強度，結 ir 以上結果可知，該糊狀銀粒子挺成 物=無銀粒子與分散狀分離，保存安定性優異，於強力 黏δ金屬製構件方面係有用的。 、 [實施例8] 4η將市售之銅粒子碎片化，製作1次粒子的平均粒徑為 雷射繞射法測定)之碎片狀銅粒子(銅表面被 0.5重㈣之硬脂酸被覆，該銅粒子具有撥水性），對剛 份之上述碎片狀銅粒子添加15份之甘油（和光純藥工業 月又伤有限公司販售之試藥’介電係數47 0)作為揮發性分 ’使用旋轉式混練機均勾混合’藉此調製糊狀銅 粒子組成物。 該糊狀銅粒子組成物於注射器内並未觀察到銅粒子盘 分散媒之分離。結果係整合示於表2。由以上結果可知/，、 該糊狀銅粒子組成物並無銅粒子與分散媒之分離，長時間 之保存安定性優異。 [實施例9] 式於實施例8中’除了取代銅粒子，使用將市售之錄粒子 碎片化而製作1次粒子的平均粒徑為6 Mm(以雷射繞射 法測疋）之碎片狀鎳粒子（鎳表面被〇8重量％之油酸被 覆，該鎳粒子具有撥水性）以外，與實施例8同樣地調製 糊狀鎳粒子組成物。該糊狀鎳粒子組成物於注射器内並未 312ΧΡ/發明說明書(補件)/96-07/96109691 28 200822991 觀察到鎳粒子I分I據夕八 ^ ^ 一刀政媒之分離。結果係整合示於表2。由 + σ果可知，该糊狀鎳粒子組成物並無鎳粒子與分散媒 刀離，長時間之保存安定性優異。 ” [實施例1 〇 ] ' 、寸00伤之市售之以沈澱法製造、^次粒子的平均粒徑 ><田身射法測定)為之粒狀銀粒子(銀表面被 ^八重里％之硬脂酸被覆，該銀粒子具有撥水性），添加 隹^之N’N~一甲基甲酿胺（和光純藥工業股份有限公司 =之試藥’介電係數38.0)作為揮發性分散媒（C)，使 疋轉式此、、東機均勻混合，藉此調製糊狀銀粒子組成物。 八f糊狀銀粒子組成物於注射器内並未觀察到銀粒子與 /苇之刀離測疋該糊狀銀粒子組成物之黏著強度，結 系i σ不於表2。由以上結果可知，該糊狀銀粒子組成 並無銀粒子與分散媒之分離’保存安定性優異，於強力 黏合金屬製構件方面係有用的。 [實施例11] 於實施例1中，除了取代节醇而使用純水（介電係數 80. 0)15份作為揮發性分散媒⑽、取代卜己烧而使用乙 醇（和光純藥工業股份有限公司販售之試藥，介電係數 24.0)3份作為揮發性分散媒（Β2)以外，與實施例i同樣 地調製糊狀銀粒子組成物。純水15份與乙醇3份之混合 溶液的介電係數為68。該糊狀銀粒子組成物於注射器内 亚未觀察到銀粒子與分散媒之分離。測定該減銀粒子組 成物之黏著強度’結果係整合示於表2。由以上結果可知， 312XP/發明說明書(補件)/96-07/96109691 29 200822991 棚狀絲子組絲並無絲子與分 定性優異’於強力黏合金屬製構件方面係有用的。保存- [比較例1 ] 於實施例丨中’除了未添加作為揮發 卜己烧，並將作為揮發性分散媒⑽之 苹定(= 份以外，與實施例1同樣地調製糊狀銀粒子組成物_ f銀粒t組成物於注射器内可觀察到銀粒子與:發= 月文媒之分離。結果整合示於表3。 [比較例2 ] 於實施例1中’除了使μ醇份作為揮發性分散 媒⑽錢卜己m份作轉發性分散媒（Β2)以外政 與實施例1同樣地調製糊狀銀粒子組成物。作為揮發性分 散媒（Β1)之14.8份节醇以及作為揮發性分散媒（Β2)之 0.2份卜己烧係擾拌混合變成為透明狀，即使靜置亦不合 分離為2層。該糊狀銀粒子組成物於注射器内可觀察到^ 粒子與揮發性分散媒之分離。結果整合示於表3。① " [比較例3] 於實施例1中，除了使用节醇〇·2份作為揮發性分散媒 (Β1)以及1-己烷14· 8份作為揮發性分散媒（β2)以外，與200822991 IX. Description of the Invention: [Technical Field] The present invention relates to a paste-like metal particle composition comprising metal particles and a volatile dispersion medium, wherein sedimentation and separation of the metal particles are suppressed, and using the paste A method of bonding metal members of metal particle compositions. [Prior Art] A conductive/thermally conductive paste formed by dispersing a metal powder such as silver, copper or nickel in a liquid thermosetting resin composition to form a conductive/thermal conductive film by heating. Therefore, it is used for formation of a conductive circuit on a printed circuit board; formation of various electronic components such as resistors and capacitors, and electrodes of various display elements; formation of a conductive film for shielding electromagnetic waves; capacitors, resistors, The formation of electrodes of a solar cell in which a semiconductor device such as (10) adheres to a substrate; the formation of an electrode of a solar cell is particularly difficult to form an electrode of a solar cell which cannot be subjected to temperature processing using an amorphous stellite semiconductor; Multilayer ceramic capacitors, layered ceramics inductors, laminated ceramic actuators, and other wafer-type ceramics, the formation of external electrodes, etc. v Private ' 'Because of the high performance of wafer parts, from wafer parts ★... Adding 'in addition to the originally required electrical conductivity, it is also required to improve the sex. Therefore, by increasing the content of metal particles as much as possible, it is desirable to improve electrical conductivity and thermal conductivity. However, the viscosity of the = will rise. In order to solve such a problem, the inventors of the present invention and the like have developed a paste composed of a volatile dispersing medium. Silver composition μ heating, 312ΧΡ/invention specification (supplement)/96-07/96109691, 〇200822991 The volatile dispersion medium will volatilize, and the silver powder will be sintered to form solid silver with extremely high conductivity and thermal conductivity. It has been found to be very useful for the bonding of metal members or the formation of conductive circuits. Therefore, a patent application is filed (Japanese Patent Application No. 2005-152827, Japanese Patent Application No. 2005-309126). However, the inventors of the present invention have also discovered that silver, A paste-like composition composed of a metal particle having a large specific gravity such as copper or nickel and a volatile dispersing medium having a small specific gravity has a large difference in specific gravity between the two, so that the metal particles are separated and settled over time. In Japanese Patent Laid-Open No. 2005-93380, there is proposed a silver ink composed of silver powder and a polyol, and a silver powder, a polyol, and a viscosity modifier (water, ketone or alcohol). In addition, it is described that the dispersibility can be improved by using a polyol and a ketone or an alcohol in combination. However, the inventors have found that a metal having a large specific gravity such as silver, copper, or nickel Since the paste-like composition composed of a polyhydric alcohol having a small specific gravity and a viscosity modifier has a large difference in specific gravity, the metal particles are separated and settled over time (Patent Document 1) Japan SUMMARY OF THE INVENTION PROBLEMS TO BE SOLVED BY THE INVENTION The inventors of the present invention have intensively studied a composition of a paste-like metal particle which does not have the above problems, that is, a time-separated separation of a metal particle and a volatile dispersion medium. It is found that a composition of a paste-like metal particle which is suppressed by the precipitation of a metal particle having a large specific gravity is suppressed. As a result, it has been found that the metal in the composition of the paste-like metal particle can be suppressed by selecting the coating agent on the surface of the metal particle and the volatile dispersion medium. Separation and sedimentation of particles 312XP/invention specification (supplement)/96-07/96109691 η 200822991, thus completing the present invention. An object of the present invention is to provide a composition of a paste-like metal particle which can prevent the separation of metal particles from a volatile dispersion medium and suppress the sedimentation of metal particles even after storage for a long period of time, that is, to preserve the stability and the difference A method of firmly bonding a metal member using the paste metal particle group-form is provided. (Means for Solving the Problem) The above object can be attained by the following invention: 0 [丨] A paste-like metal particle composition comprising: (A) 100 parts by weight of metal particles, which is an average particle diameter 〇· 〇〇丨~“# m, the surface is coated with water-based organic matter; and (B) 3 to 30 parts by weight of a volatile dispersion medium; the volatile dispersion medium (B) contains a volatile dispersion medium having a different dielectric constant ( B1) and the volatile dispersing medium (B2), and the volatile dispersing medium (B1) and the swaying property are the mixing ratio of the medium (B 2 ) which is incompletely compatible at normal temperature. [2] as in [1] a paste-like metal particle composition, wherein the water-repellent organic substance is a hydrazine fatty acid, a higher fatty acid decylamine or a higher fatty acid ester, and the metal of the metal or the particle (A) is gold, silver, copper, nickel, tin, [3] The composition of the paste metal particles according to [2], wherein the metal particles (A) are silver particles coated with higher fatty acids. [4] The paste metal of [1] a particle composition in which a volatile dispersing medium-(B1) and a volatile dispersing medium (B2) are selected from the following groups : water, volatile 1 alcohol, volatile 1-alcohol with ether linkage, volatile polyol, volatile hydrocarbon, volatile ether, volatile fatty acid ester, volatile ketone, volatile fat l S basket amine Volatile aliphatic amine and alkyl base; and, the volatile component 312XP / invention specification (supplement) / 96-07/96109691 8 200822991 solvent (B1) and the volatile dispersion medium (82) at 25Ct The difference in the dielectric constant is 2.0 or more. [5] The composition of the paste metal particles according to [1], wherein a mixing ratio of the volatile dispersing medium (β1) to the volatile dispersing medium (B2) is 98·· 2~2 ·· 98. [6] The composition of the paste-like metal particles of [4], wherein the mixing ratio of the volatile dispersing medium (Β1) to the volatile dispersing medium (β2) is 98 ·· 2 2 · 98. [7] A method for bonding a metal member, characterized in that the paste-like metal particle composition of any one of [1] to [6] is interposed between a plurality of metal members, The volatile dispersing medium is volatilized by heating, by pressurizing and applying ultrasonic vibration, or by applying pressure and heating and applying ultrasonic vibration, and the metal particles are dispersed. The plurality of metal members are bonded to each other by the sintering of the plurality of metal members. [8] A paste-like metal particle composition characterized by comprising: (Α) 1 part by weight of metal particles, The average particle size 〇· 001~50// ra, the surface is coated with water-based organic matter; and (C) 3 to 30 parts by weight of the volatile dispersion medium, which has a dielectric constant of 30 to 75 at 25 ° C, is not rejected Metal particle (A). [9] A paste-like metal particle composition such as [8], wherein the water-repellent organic substance is a south fatty acid, a higher fatty acid guanamine or a higher fatty acid ester, and a metal particle (A) metal It is made of gold, silver, copper, handle, record, tin, Ming or these alloys. [10] The paste-like metal particle composition according to [9], wherein the metal particles (a) are silver particles coated with a higher fatty acid. [11] A paste-like metal particle composition such as [8], wherein the volatile dispersion medium (C) is a volatile polyol, a dimercaptodecylamine or a volatile monohydric alcohol water 312XP/invention specification (supplement) ) /96-07/96109691 9 200822991 Solution. [12] A method for bonding a metal member, characterized in that a paste-like metal particle composition of any one of [7]~uchuan is interposed between a plurality of members by a domain, by a side Pressurizing and applying ultrasonic vibration, or: Hunting by pressurization and heating and applying ultrasonic vibration, volatilizing the volatile dispersion medium (6), and sintering the metal particles (A) with each other, thereby causing the plurality of metal members to mutually Bonding. (Effect of the Invention) The paste-like metal particle composition of the present invention can be separated from a volatile dispersion medium (8) having a small specific gravity and a metal particle having a large specific gravity (A) even if it is stored for a long period of time. ) a precipitation, can maintain a uniform paste state. According to the bonding method of the present invention, the paste-like metal particle composition between the metal members is volatilized by heating by heating, and the metal is heated at a temperature higher than the sintering temperature of the metal particles (A). The particles (a) are sintered to each other to form a solid, and a plurality of metal members can be firmly bonded to each other. [Embodiment] The paste-like metal particle composition of the present invention is characterized in that it contains (A) 100 parts by weight of metal particles having an average particle diameter of 〇〇〇1 to 5〇#m, and the surface is dialed. The water-based organic material is coated; and (B) the volatility of 3 to 3 parts by weight of the volatile medium is a political medium, and the volatile dispersion medium (B) contains a medium having a different dielectric coefficient as a political medium (B1) and a volatile dispersion medium. (B2), and the volatile dispersing medium (b1) and the volatile dispersing medium (B2) are in a mixing ratio which is incompletely compatible at normal temperature. 312XP/Invention Manual (Supplement)/96-07/96109691 10 200822991 The surface of the particle (A) must be covered with water-based organic matter. The organic material is preferably excellent in lubricity, and is preferably a higher fatty acid, a higher fatty acid metal (except for the alkaloids), a higher fatty acid guanamine, and a higher fatty acid ester. The amount of the water-repellent organic material to be coated varies depending on the particle diameter, specific surface area, shape, and the like of the metal particles, and is preferably from 0. 01 to 3 by weight of the metal particles, more preferably from 2 to 2% by weight. If it is too small, the stability is lowered, and if it is too large, the heat sinterability is lowered. The material of the particle (Α) is ® 常 at normal temperature, and it can be sintered by twisting or heating and applying ultrasonic vibration, and examples thereof include gold, silver, copper, tin, and the like. Among these, in terms of silver, copper, self-heating sinterability, thermal conductivity, and electrical conductivity, the bismuth silver particles may have only a part or all of the surface thereof being silver oxide. The average particle size of the sub (Α) is 〇〇〇1~5〇^. The average particle diameter / which is obtained by the field diffraction diffraction type particle size distribution method, if the average particle diameter exceeds 5 〇 (10), it becomes difficult to prevent gold == Therefore, it is preferable that the average particle diameter is smaller, and 2 One is the case, ^= and the size of the stomach is less than 0々m. So 'to. The stability of the storage is reduced. The shape of the particles (1) is spherical, and substantially spherical. The gold M ^ has a substantially spherical shape of a substantially cubic shape, and is preferably a shape of a chip or the like. From the viewpoint of preservation stability, it is especially preferred that the silver particles produced by the reduction method have a variety of methods for producing the silk of the original method, but the system is a 312XP/invention specification (supplement) pulse _ 61〇9691 Μ 200822991 ^ Adding a hydrogen oxy-aqueous solution to a silver sulphuric acid reading solution to prepare silver oxide, and adding eight to an aqueous solution of a reducing agent such as brown horse, thereby reducing silver oxide to form silver particles, and then performing Washed, filtered, dried, etc. By dispersing the metal particles attached to the water-based organic material, it is possible to add a water-repellent organic substance to the granular metal particles, for example, and pulverize it by ball milling or the like, and it is possible to make clothes (see Japanese Patent Publication No. 4,6971, Open [20004341 07 [〇〇〇4]). r - a granular organic material such as a granular metal particle and a higher fatty acid, a higher fatty acid metal salt (except a base to a genus salt), a two-stage fatty acid ester, a higher fatty acid guanamine, etc., and a rotary drum is placed together with a ball made of pottery In a device (for example, a ball mill), metal particles are physically patted by a ball, whereby the chips can be easily processed into pieces (scales). In this case, a water-repellent organic substance such as a high-grade fatty acid, a higher fatty acid metal salt (except an alkali metal salt), a higher fatty acid ester, or a higher fatty acid guanamine for improving lubricity is attached to the chip-shaped metal particles. Examples of such higher fatty acids include lauric acid and nutmeg (k, palmitic acid, stearic acid, oleic acid, linoleic acid, and linoleic acid, preferably higher saturated fatty acids. As such higher saturated fatty acids, Examples of lauric acid, myristic acid, palmitic acid, and stearic acid are used. The surface of the fragmented metal may be coated with more than half of such higher fatty acid, but it is preferably coated. The metal surface is coated with a water-repellent organic substance. Metal particles, which show water repellency. If the amount of water-based organic matter adhered is too small, the metal particles are easily separated and sedimented. If too much, the sinterability is lowered. Therefore, the amount of water-repellent organic matter is preferably 〇·01~3 %, more preferably 〇. 1~1%. The amount of water-based organic matter adhered can be determined by a general method. For example, it can be exemplified by heating in the nitrogen 312 edge/invention specification (supplement)/96-07/96109691 12 200822991 The method of measuring the weight reduction by dialing the boiling point of the aqueous organic substance is to 'heat the metal particles in the oxygen gas stream, and convert the carbon attached to the water-repellent organic substance of the metal particles into A method of quantitatively analyzing carbon oxide by infrared absorption spectroscopy. The metal particles (A) coated with a water-repellent organic substance can also be produced by a general method, for example, by immersing metal particles in a water-repellent organic substance/ In the trough liquid, the metal particles are taken out and dried to produce. The volatile dispersing medium (B) is composed of a volatile dispersing medium (B1) having a different dielectric constant and a volatile dispersing medium (B2), and ^ and volatility The dispersing medium (10) is a ντ compound which is incompletely soluble at normal temperature. Whether it is not completely compatible, it can be determined by the following method. That is, the volatile dispersing medium (Bl) is mixed and mixed in a glass container. The medium (10) is allowed to stand until the bubble disappears, and is visually observed. When the separation is turbid, it can be judged as incompatible. When one layer is transparent, it can be judged to be compatible. n : Volatile dispersing medium (10) and volatilization The dispersing medium (10) is dissolved and becomes a tick-like shape: 'The metal ion in the paste-like metal composition (=the biochemical method prevents the sedimentation phenomenon. The mixing ratio of the volatile dispersing medium (10)' is not completely compatible The ratio is preferably in the range of 99: 2 to 2: 99. And the ratio of the paste-like metal particle composition of the present invention to the k-type or the heating/ultrasonic vibration sinterability. The solvent is not non-volatile and must be volatile/two or four agents' in the case of metal particles (A) 312XP / invention manual (supplement) / 96-07/96109691 13 200822991 for silver particles, If it is easy to sinter, it is easy to use it as a volatilization of the medium, then the silver particles become volatile. (4) The boiling of 5 doses, the adhesive 'Therefore the above limitation. If the boiling point is less than 6 (TC, 2 6 〇 C) ～3〇〇C is preferred. The reason for this is that the volatilization of the material during operation is likely to remain in the (4) paste-like metal particle-constitutive dispersion medium (8). '.300 c', even if heated, volatilizes volatile volatile compounds (β), which are volatile volatile organic compounds; volatile organic compounds consisting of the original, and hydrogen atoms; a volatile organic compound composed of a dioxygen atom; a volatile organic compound & oxygen atom and a liquid composed of a carbon atom and a nitrogen atom of an atom. ...has a branch of compound 荨. Specifically, at room temperature, volatile monohydric alcohols such as hexanol, heptyl alcohol, naphthol, ethyl fresh, propanol, butanol, pentanol, hexanol, epigalol, and decyl alcohol; Ethylene glycol monomethyl A, based on carbaryl, methyl carbitol, ethylene glycol monoethyl bis = carbitol alcohol ethylene glycol monopropyl _ (propyl celecoxib, propyl h Glycol monobutyl wire (butyl cyproterone, butyl carbitol), one: alcohol monomethyl _, methyl methoxy butanol, etc. Volatile aromatic alkyl alcohols such as alcohol; volatile polybasic alcohols such as ethylene glycol, propanol and glycerin; volatile aliphatic hydrocarbons such as low-grade paraffin wax and low-grade paraffin; volatile aromatics such as toluene and xylene Group II 'acetone, mercaptoethyl ketone, decyl isobutyl ketone, cyclohexanone, diacetone • (4~hydroxy-4-indolyl-2-pentanone), 2-octanone, isophorone ( 3,5,5-tridecyl-2-cyclohexene-one ketone), diisobutyl ketone (2,6-didecyl _4-heptane ^ 312 ΧΡ / invention specification (supplement) / 96- 07/96109691 14 200822991 and other volatile aliphatic ketones; ethyl acetate (ethyl vinegar Ester), butyl acetate, ethoxylated ethane, decyl butyrate, decyl hexanoate, decyl octoate, decyl decanoate, decyl cyproterone acetate, propylene glycol monodecyl ether acetate, etc. Volatile aliphatic carboxylic acid ester; Sifufunan, dipropyl _, ethylene glycol dimercapto bond, ethylene glycol diethyl ether, ethylene glycol dibutyl ether, butanediol didecyl Volatile aliphatic ethers such as ether and ethoxyethyl ether; low molecular weight volatile anthrone oils and volatile organic modified anthrone oils; volatilization of acetamide, hydrazine, decyl decyl hydrazine, etc. a carboxylic acid decylamine; a volatile first-grade aliphatic amine such as mercaptoamine, ethylamine, propylamine or ethylenediamine; a volatile secondary aliphatic amine such as dimethylamine or diethylamine Volatile tertiary aliphatic amines such as tridecylamine and triethylamine; other volatile aliphatic amines; volatile alkyl nitriles such as acetonitrile and propionitrile. Water is preferably pure water, and its electrical conductivity is better. Preferably, it is l〇〇/zS/cm or less, more preferably 10 // S/cra or less. The method for producing pure water can be exemplified by an ion exchange method, a reverse osmosis method, or a steaming crane method by a general method. The dispersion medium (B1) and the volatile dispersion medium (B2) must have a dielectric constant difference of 2 or more at 25 ° C from the above-mentioned volatile medium (B), preferably 3 or more, more preferably selected. 5 or more. As the volatile dispersing medium (B1), it is preferred to select water of a dielectric constant surface at 25 ° C, a volatile monohydric alcohol, a volatile polyol, a volatile aromatic alcohol, an alcohol, N, N-dimercaptodecylamine, volatile aliphatic amine, volatile aliphatic _, volatile aliphatic carboxylic acid ester or volatile aliphatic ketone, as volatile dispersion medium (B2), preferably selected 25° Volatile aliphatic ether, volatile aliphatic carboxylic acid ester, volatile under C, which is 2 or more smaller than volatile media (B1) (preferably less than 3, more preferably less than 5) Aliphatic 312XP / Inventive Specification (Supplement) / 96-07/96109691 15 200822991 Ketone, volatile aliphatic hydrocarbons, volatile aromatic hydrocarbons or volatile (tetra) oils. In this case, if the difference between the electric coefficients of the volatile dispersion medium (8) and the volatile dispersion medium (10) at 25 ° C is 2 or more (preferably 3 or more, more preferably 5 or more), The organic compound of the same kind. The volatilizing knife (β) and the volatile dispersing medium (B2) are in the Μ. The dielectric of the γ number is 2, the compatibility of the two volatile dispersion media is changed. It is easy to prevent the separation and sedimentation of the metal particles (A) in the paste-like metal particle composition. The difference in dielectric coefficient at 25 C is 2 or more (preferably 3 or more, more preferably 5 or more), although The volatile dispersion medium (Μ) and the volatile dispersion medium (B2) are still compatible to some extent, but must not be completely compatible. Also, when mixed with the metal particles (A), the volatile dispersion medium (B1) The volatile dispersing medium (B2) must be used in a certain degree of compatibility, but it must be a mixing ratio that is not completely compatible. Alternatively, two or more kinds of volatile dispersing media (B1) and (B2) may be used together. It must be a mixing ratio that is incompatible when (B1) and (B2) are mixed. The amount of the volatile dispersion medium (B), that is, the volatile dispersion medium (B) 1) The total amount of the fish volatile dispersion medium (B2) is 3 to 30 parts by weight per 1 part by weight of the metal particles (A), which is sufficient for the metal particles (A) to be paste-like at normal temperature. The composition of the paste-like metal particles of the present invention may contain a small amount or a small amount of a non-metallic powder other than the metal particles (A), a metal compound, a metal complex, and a shake as long as it does not deviate from the object of the present invention. Additives such as varnish, stabilizer, coloring agent, etc. Μ The paste-like metal particle composition of the present invention can be easily fabricated by placing the following components in a mixer, stirring and mixing until uniformity is present: 312 ΧΡ / Inventive specification (supplement)/96-07/96109691 16 200822991 (A) 100 parts by weight of metal particles having an average particle diameter of ~1 to 5 〇//m, the surface being coated with water-repellent organic matter; and (B) 3 to 3 parts by weight of the volatile knife medium. The volatile dispersion medium (βΐ) and the volatile dispersion medium (β2) may be premixed to have a certain degree of compatibility, or may not be completely compatible. Metal particles (Α) are mixed. Alternatively, volatile dispersion media may be mixed separately. (β1) and the volatile dispersing medium (Β2). The paste-like metal particle composition of the present invention is a metal particle (a mixture of the gossip and the volatile dispersing medium (8), which is a paste at normal temperature. In addition, the paste-like system contains In the form of a cream, it can be ejected from a syringe or a nozzle into a thin line shape, and can be easily applied by a metal mask. Features of the paste-like metal particle composition of other embodiments of the present invention It is composed of (A) 100 parts by weight of metal particles having an average particle diameter of 0.001 to 5 〇em, and the surface is coated with a water-repellent organic substance; and a part by weight of a volatile dispersion medium having a dielectric constant of 25 Å. 3〇~M. Since the metal particles (Α) are coated with a water-repellent organic substance, separation and sedimentation can be suppressed by using a volatile dispersing medium having a dielectric constant of 30 to 75 in combination. If the metal particles are not coated with the water-repellent organic substance, separation and sedimentation cannot be suppressed even when used in combination with the volatile solvent (C). The metal particles (A) are as described above. The volatile dispersing medium (C) may be selected from the group consisting of a 25 ° C dielectric constant of 30 to 75: a volatile organic compound composed of a carbon atom, a hydrogen atom and an oxygen atom; and a carbon atom, a hydrogen atom and a nitrogen atom; The volatile constituents of the atom are composed of a volatile compound such as a carbon atom, a hydrogen atom, an oxygen atom and a nitrogen atom. Specifically, a volatile monohydric alcohol, a volatile polyol, a volatile lower aliphatic carboxylic acid, which is available from 25t: a dielectric constant of 312 ΧΡ / invention specification (supplement) / 96_〇7/96ΐ〇9691 17 200822991 Aqueous solutions of guanamine, volatile alkyl nitriles and volatile alcohols (eg volatile monohydric alcohols, volatile polyols) are selected. Examples of such a volatile dispersing medium include volatile monohydric lower alcohols such as methanol; aqueous solutions of volatile monohydric lower alcohols (for example, ethanol), volatile polyhydric alcohols such as ethylene glycol, propylene glycol, and glycerin; acetamidine and dimethyl A volatile alkyl nitrile such as decylamine or a volatile lower aliphatic carboxylic acid decylamine, acetonitrile or propionitrile. Among these, a polyol having a dielectric constant of 3 〇 to 7 Å is preferred. Further, when two or more kinds of dispersion media are used in combination, the mixture may have a dielectric constant of 30 to 75. The amount of the volatile dispersion medium (C) is 30,000 weight loss per part by weight of the metal particles (A), and is the above-mentioned paste metal particles required for the paste formation of the metal particles (a). The composition may contain a small amount or a small amount of an additive such as a non-metallic body, a metal compound, a metal complex, a shaker, a stabilizer, a colorant or the like other than the metal particles, without departing from the object of the present invention. The above-mentioned paste-like metal particle composition of the present invention can be easily produced by placing the following components in a mixer and stirring and mixing until uniformity is present: (A) 100 parts by weight of metal particles, which are average particles 〇 〇 〜 1~5〇#❿, the surface is coated with water-based organic matter; and (c) 3 to 3 parts by weight of volatile dispersion medium. The above-mentioned paste-like metal particle composition of the present invention is a mixture of metal particles (A) and a volatile dispersing medium (C), and is a paste at normal temperature. In addition, the paste also contains a cream. By paste formation, it can be ejected from a syringe or a nozzle into a thin wire 312XP/invention specification (supplement)/96-07/96109691 18 200822991, and it can be easily printed and coated with a metal mask. The above two kinds of paste metal particle compositions of the present invention are volatilized via a twisted volatile dispersion medium. In the above-mentioned two types of paste-like metal particles of the present invention, the temperature is increased to a temperature higher than the sintering temperature of the metal particles, and the ultrasonic vibration is applied while applying pressure, in particular, while applying pressure and heating sub-application super The acoustic vibration causes the volatile dispersing medium (B) or the volatile dispersing medium and (C) to be volatilized, and the metal particles (A) are sintered to each other to form a solid-shaped metal excellent in strength, electrical conductivity, and thermal conductivity. It is also possible to apply pressure when the paste metal particle composition is heated. At this time, the volatile dispersing medium (8) or the volatile dispersing medium (6) may be volatilized 'then sintering the metal particles (a), and the volatile dispersing medium (8) or the volatile fraction (4) (6) may be volatilized, and (4) the sintered metal particles (A) are mutually . Especially in the case where the metal particles (A) are silver particles, since the silver originally has high strength and extremely high electrical conductivity and thermal conductivity, the sintered particles of the silver particles of the present month are also high in strength and extremely high. Electrical conductivity and thermal conductivity. The heating temperature at this time may be a temperature at which the silver particles can be volatilized by volatilizing the volatile dispersing medium (8) or the volatilizing medium (C), and is usually at least a loot or more, preferably 15 (TC or more. However, If it exceeds 4 ° C, the volatile dispersing medium will evaporate in a Buddha's way, which may adversely affect the shape of the solid metal. Therefore, it must be 4 〇 or less, preferably 300 ° C or less. When the metal particles (A) which are not easily sintered are heated, the ultrasonic vibration is applied while being pressurized, or the ultrasonic vibration is applied while being pressurized, heated, and ultrasonic vibration is applied. The frequency of the ultrasonic vibration is 2 kHz or more. It is preferably 〇 kHz or higher. The upper limit is not particularly limited, and is about 5 kHz in terms of device capability. Also, 312XP/Invention Manual (supplement)/96-07/96109691 19 200822991 Ultra: amplitude of wave vibration It is preferably 0. 1~40//m, more preferably 0.320//m, and more preferably 〇·5~. In addition, in order to transmit ultrasonic vibration to the paste metal particle composition Preferably, the transmitting portion of the ultrasonic vibration is directly abutted The composition of the paste-like metal particles, or the covering portion of the ultrasonic vibration is abutted by a covering material made of a material that does not easily absorb the ultrasonic vibration, and the abutting force of the composition of the paste-like metal particles is preferably 〇 · 9kPa (0. 09gf/mm2) or more, more preferably 9kPa (j·92gf/_2) or more, especially preferably 39kpa (3·98gf/_2) or more, and the upper limit of the abutting pressure is the pressure of the member that does not break the adhesion. The heating temperature in the case of sintering, heating, and applying ultrasonic vibration, as long as it is higher than normal temperature, and the volatile dispersing medium (B) or the volatile dispersing medium (C) can be volatilized and the metal particles can be The temperature of the sintering may be sufficient. However, if the heating temperature exceeds 400 ° C, the volatile dispersion medium (B) or the volatile dispersion medium (C) may evaporate in a sudden boiling manner, which may adversely affect the shape of the solid shape metal. The temperature is preferably 400 Torr or less and less than the melting point of the metal particles (A), and is preferably 3 Å or less. The shape of the solid metal obtained by sintering the metal particles (A) is not particularly limited. Example sheet, film shape a strip shape, a line shape, a disk shape, a block shape, a dot shape, or an irregular shape. The above two types of paste metal particle compositions of the present invention are heated, or by applying pressure and applying ultrasonic vibration, or It is a method of pressurizing, heating, and applying ultrasonic vibration to volatilize the volatile dispersing medium (β) or the volatile dispersing medium (C), and to sinter the metal particles. The strength and electrical conductivity and thermal conductivity of the solid metal formed by sintering. Excellent, with metal structure for contact 312ΧΡ/Invention manual (supplement)/96-07/961〇9691 20 200822991 : : := Substrate, silver plated metal substrate, copper substrate, nickel plated substrate, tinned metal substrate, etc. The metal base layer=adhesiveness of a metal portion such as an electrode on an insulating substrate is useful for bonding a substrate or an electronic component having a metal portion, an electronic device, or an electric component, an electric device, or the like. The bonding can be exemplified by the bonding of the Japanese and Japanese film parts such as electric power and electric resistance to the circuit substrate; the bonding of the semiconductor wafer and the lead frame or the circuit substrate; and the binding of the CPU chip to the cooling plate. After the above-mentioned two types of paste-like metal particle compositions of the present invention are sintered, since there is no residual knife medium, there is no need to wash them, but they may be washed with water or water. Since the above two kinds of paste-like metal particle compositions of the present invention contain a volatilization medium (8) or a volatile dispersion medium (6), they are preferably stored in a closed valley. It can also be stored in a refrigerator for the purpose of improving the storage stability. The storage temperature can be exemplified by 1 〇 °c or less. [Examples] Examples and comparative examples of the present invention are disclosed below. In the examples and comparative examples, the term "parts" means "parts by weight". Method for measuring the amount of water-repellent organic matter in metal particles, method for measuring dielectric constant of volatile dispersion medium, method for measuring separation of metal particles and volatile dispersion medium during storage of paste-like metal particle composition, and borrowing method The adhesive strength of the solid-shaped metal produced by heating the paste metal particle composition or performing ultrasonic ultrasonic compression bonding was measured by the following method. Further, the temperature in the case where it is not particularly described is 25 °C. 312XP/Invention Manual (Supplement)/96-〇7/96109691 200822991 [Water-based organic matter amount] The measurement was carried out by the following method using the πίΑ method. The metal particles were heated to 5 〇rc at a rate of io:c/: in a stream of nitrogen gas, and kept at 5 Torr (rc for 1 hour. Definition [weight before heating - weight after heating] / [weight before heating] xl 〇〇 = amount of water-repellent organic matter (unit %) [Dielectric Coefficient] The measurement was carried out using a liquid dielectric constant measuring device (manufactured by Scientific Co., Model No. 870). <[Separation of metal particles from volatile dispersion media] Composition of paste metal particles! Insert the syringe 3 (inner diameter 12 mm, length 55 mm, internal volume 5 cc, manufactured by EFD) to which the front end cover 2 is attached, and install the piston 4 so that the front end of the syringe 3 faces downward to a height of 3 mm, and finally install the tail. The end cap 5 is sealed. The front end of the syringe 3 was held downward and held vertically, and allowed to stand for 24 hours. The thickness (mm) of the volatile dispersing medium layer in the upper portion of the paste-like metal particle composition 1 in the syringe 3 was measured. [Adhesive strength A] A paste-like metal particle composition (coated area: 5 imn X 5 inm) was applied to a silver-plated copper plate having a width of 25 mm x 75 and a thickness of Ιππη using an iOOp thick metal mask, and a width of 5 mm x length 5 mm x thickness was mounted thereon. After the silver wafer of 〇5 coffee, the silver wafer was adhered to the silver-plated copper plate by heating in a forced circulation oven at 2 Torr (rc). The test body for measuring the adhesion strength thus obtained was attached to the die shear. Force (Die讣 /) strength tester, the die shear tool of the die shear strength test machine, press the side of the silver wafer at a speed of 23mm / minute. Silver wafer and plating 312XP / invention manual (Supplement)/96-07/96109691 22 200822991 The weight of the bond between the silver and copper plates is the bond strength when the shear is broken (unit: kgf). In addition, the adhesion strength test is performed 3 times, with the average value being Adhesive strength A. - [Adhesive strength B] Using a 100/zm thick metal mask, apply a paste-like metal particle composition (coated area: Smmdnnn) to a silver-plated copper plate with a width of 25 legs and a length of 75 mmx and a thickness of 1 mm. It has a width of 5mmx 5 χ χ 〇 5 5 5 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖 咖Under the condition of a pressure of 1〇〇N/cm2, the pressure-sensitive adhesive portion (probe) of the ultrasonic thermal pressure bonding device is abutted against the upper portion of the silver wafer of the precursor for adhesion strength measurement, and ultrasonic vibration is applied thereto. One side is pressed at a temperature of 20 (TC for 3 sec. The adhesive strength thus prepared is mounted on a die shear strength tester, and the die shear of the test head is measured by the shear strength of the die. The force cooker presses the side of the silver wafer at a speed of 23 mjn/min. The load when the bond between the silver wafer and the silver-silver copper plate is shear-damaged is the bond strength (unit: in.., in addition, the adhesion strength test system) Three times, the average value was sticky [Example 1] Commercially available silver particles produced by a reduction method were fragmented to prepare i-order particles: particle size was 3. 〇A m (determined by laser diffraction method) ) the fragmented silver particles water ini 5 wt% hard Acid-coated, the silver particles have 12 parts of benzyl alcohol added to the above-mentioned fragmented silver particles (and, first, the reagents sold by Yule Industrial Co., Ltd., dielectric constant 13. (〇作312XP/ Inventive specification (supplement)/96-07/96109691 23 200822991 is a volatile dispersion medium (B1) and 3 parts of 1-hexane (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant 2·〇) As a volatile dispersing medium (B2), it was uniformly mixed using a paddle stirrer, thereby preparing a paste silver particle composition. The mixture of 12 parts of benzyl alcohol as the volatile dispersion medium (B1) and 3 parts of 1 part of the volatile knife medium (B2) was incompatible. When the two are stirred and mixed, a white turbidity phenomenon occurs, and when left to stand, it is immediately separated into two layers. The paste silver particle composition was not observed to separate the silver particles from the volatile dispersion medium in the syringe. The results of measuring the adhesion strength of the pasty silver particle composition are shown in Table i. From the above results, it is understood that the paste silver particle composition has no separation of silver particles and a volatile dispersing medium, and is excellent in storage stability, and is useful for strongly bonding metal members. [Example 2] In the Example ', in addition to the substitution of the silver particles, the copper particles of the returned material were fragmented to prepare a fragmented copper particle having an average particle diameter of the i-th particle of Up (with a laser diffraction if). The copper-like copper particle composition was adjusted in the same manner as in Example i except that the copper surface was replaced by G. 5 wt% stearic acid = 'the copper particles had water repellency. The paste copper particle composition was observed in a syringe and the separation of the copper particles from the volatile dispersion medium was observed. The results are shown in the above results. The separation of the hair-forming dispersible medium is observed. [Example 3] The paste-like copper particle composition was excellent in storage stability without copper particles and the growth of the day. Fragmentation of commercially available nickel particles to produce primary particles with an average particle size of 312XP / invention specification (supplement) / 96-07/96109691 200822991 6. ° = laser diffraction method) 12 copies of NN-_ w A w (Waguang Pure Pharmaceuticals Co., Ltd. sells 'methantamine and 3 parts of hexamethylene: = = : sex: a mixture of 3 parts of the medium (10) The stool was immediately separated into 2 layers, and a white turbidity phenomenon occurred. 'The static wave was::, the particle composition was not observed in the syringe. The separation of the recorded particles and the knife was observed. The result is shown in the table by the above == The paste composition particle composition is excellent in storage stability between the unrecorded particles and the volatile dispersion knife. [Example 4] Commercially available silver particles produced by a reduction method are fragmented to prepare a secondary particle. : the surface of the fragmented silver silver having an average particle diameter of 3.0/^ (measured by a laser diffraction method) is coated with 0.5% by weight of stearic acid, the silver particles having water repellency), and 100 parts of the above-mentioned fragments Adding a portion of bis (2-methoxyethyl) ether in the form of silver particles (a reagent sold by Wako Pure Chemical Industries Co., Ltd., Electric coefficient 5.6) as a volatile dispersion medium (B1) & 4 parts of ethylene glycol (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant 39. 〇) as a volatile dispersion medium (B2), Mix evenly with a paddle stirrer 312XP/Invention Manual (supplement)/96-07/96109691 25 200822991 B. 14 Soil (4) 11 parts of a mixture with 11 parts of ethylene glycol as a volatile dispersing medium (B2) # ^ ^ , ^ Ιθ . The ratio of work ', phase bath. When the two were stirred and mixed, white turbidity was observed, and when left to stand, they were immediately separated into two layers. The composition of the paste-like silver particles was in the body of the body, crying, and taking the matter, and the separation of the silver particles from the volatile dispersion medium was not observed in the main emitter. The results of the measurement of the adhesion strength of the composition of the silvery particles of yttrium and yttrium were shown in Table 1. From the above, it is known that the paste silver particle composition has no separation of the silver particles and the volatile component (4), and is excellent in storage stability, and is useful for strongly bonding metal members. [Example 5] Granular silver particles manufactured by the shoji method and having an average particle diameter of μ particles of 1·1//ιη (measured by a laser diffraction method) were commercially available (the silver surface was 1.5 weight) % stearic acid coated, the silver particles have water repellency), and 14 parts of 1,2-diethoxymethoxyethane (a reagent sold by Wako Pure Chemical Industries Co., Ltd.) has a dielectric constant of 7. 3 As a volatile dispersing medium (βι) and 2, Isozol 300 (a mixture of isoparaffin sold by Nippon Oil Co., Ltd., dielectric constant 2.1) as a volatile dispersing medium (β2), using a paddle stirrer The mixture was uniformly mixed to thereby prepare a paste silver particle composition. The mixture of 14 parts of 1,2-diethoxymethoxyethane as a volatile dispersing medium (Β1) and 2 parts of Is〇z〇i 300 as a volatile dispersing medium (Β2) is incompatible = ratio. When the two were stirred and mixed, white turbidity was observed, and when left to stand, they were immediately separated into two layers. The paste silver particle composition was not observed to separate the silver particles from the volatile dispersion medium in the syringe. The adhesion strength of the paste silver particle composition was measured 312XP/invention specification (supplement)/96-07/96109691 26 200822991 degree, and the results are shown in Table 1. From the above results, the paste silver particle composition is The separation of the silver-free particles from the volatile dispersion medium is excellent in storage stability and is useful for strongly bonding metal members. [Example 6] In Example 5, in addition to being a volatile dispersing medium (β1)-substituted hydrazine, 2-diethoxycarbonyl bromide was used and methyl-n-hexyl group was used (Wako Pure Chemical Industries Co., Ltd.) In the same manner as in Example 5, a paste was prepared in the same manner as in Example 5 except that 14 parts of the reagent "dielectric coefficient of 12.2" were sold and replaced with a volatile dispersing medium (B2) and pure water (steamed water, a dielectric constant of 8 Å) was used. Silver particle composition. As a mixture of the volatilization = the methyl n-hexyl group of the solvent (10) and the mixture of 2 parts of the pure water as the volatile dispersing medium (B2), the incompatible mixture causes white turbidity. Taxation The composition of the paste-like silver particles was not observed in the syringe. The adhesion strength of the paste silver particle composition was as shown in Table 1. It can be seen from the above results that the paste-like silver particles are not separated from the volatile dispersion, and the stability is different, and the structure is strongly bonded to the metal member [Example 7] The silver particles produced by the reduction method were fragmented, and the average particle diameter of the prepared cloth was 3.0/zm (was wound by a laser, and the surface of the seed was 0.5% by weight of the hard-fat silver-like silver particles). . The above-mentioned pieces of the second quilt: plus ^ (the reagents sold by Wako Pure Chemical Industries Co., Ltd. plus eight 15, ethylene glycol as a volatile dispersion medium (c) 吏:; | electric coefficient 39. 0) The rotary kneading machine is uniformly mixed, and the composition of the paste silver particles is prepared by the 312XP/invention specification (supplement)/96-07/96109691 27 200822991. Eight:: Silver: The composition of the sub-component is not observed in the syringe. The adhesion strength between the silver particles and the composition of the paste-like silver particles is observed. The results of the above-mentioned ir-ir silver particles are known to be silver-free particles. It is separated from the dispersion and has excellent preservation stability, and is useful for strong viscous δ metal members. [Example 8] 4η fragmented copper particles were obtained by fragmenting commercially available copper particles, and the average particle diameter of the primary particles was measured by a laser diffraction method) (the copper surface was coated with 0.5 weight (four) of stearic acid, The copper particles have water repellency), and 15 parts of glycerin is added to the above-mentioned fragmented copper particles (the reagent of the company sold by Wako Pure Chemical Industries, Ltd., and the dielectric coefficient of 47 0) is used as a volatile component. The rotary kneading machine is hooked to mix 'by this to modulate the composition of the paste copper particles. The paste copper particle composition did not observe separation of the copper particle disk dispersion medium in the syringe. The results are shown in Table 2. As a result of the above, it is understood that the paste copper particle composition does not have separation between the copper particles and the dispersion medium, and is excellent in storage stability for a long period of time. [Example 9] In Example 8, except for the substitution of copper particles, fragments obtained by fragmenting commercially available recording particles to produce primary particles having an average particle diameter of 6 Mm (measured by a laser diffraction method) were used. A paste nickel particle composition was prepared in the same manner as in Example 8 except that the nickel particles were coated with 8 wt% of oleic acid and the nickel particles were water-repellent. The paste nickel particle composition was not isolated in the syringe. 312 ΧΡ / invention specification (supplement) / 96-07/96109691 28 200822991 The separation of nickel particles I was observed. The results are shown in Table 2. It is known from the + σ fruit that the paste-like nickel particle composition does not have nickel particles and a dispersing medium, and is excellent in storage stability for a long period of time. [Example 1 〇 ] ', 00 00 wounds are commercially available by precipitation method, and the average particle size of the secondary particles ><Ten body shot method; the granular silver particles (the silver surface is covered with 8% of the stearic acid, the silver particles have water repellency), and the N'N~methylmethanamine is added (Wako Pure Chemical Industries Co., Ltd. = test reagent 'dielectric coefficient 38.0) As a volatile dispersing medium (C), the mash-type and the east machine were uniformly mixed to prepare a paste-like silver particle composition. The adhesion of the silver particles and the knife of the paste to the composition of the paste silver particles was not observed in the syringe of the eight-paste silver particle composition, and the relationship i σ was not in Table 2. From the above results, it is understood that the composition of the paste silver particles is not separated from the dispersion medium by the silver particles. The storage stability is excellent, and it is useful for strongly bonding metal members. [Example 11] In Example 1, except for the substitution of the phenol, 15 parts of pure water (dielectric coefficient 80. 0) was used as the volatile dispersion medium (10), and ethanol was used instead of the hexahydrate (Wako Pure Chemical Industries Co., Ltd.) A paste-like silver particle composition was prepared in the same manner as in Example i except that the reagents sold by the company had a dielectric constant of 24.0) and 3 parts as a volatile dispersion medium (Β2). A mixture of 15 parts of pure water and 3 parts of ethanol has a dielectric constant of 68. The paste silver particle composition was not observed to separate the silver particles from the dispersion medium in the syringe. The results of measuring the adhesion strength of the silver-reduced particle composition are shown in Table 2. From the above results, it is known that the 312XP/invention specification (supplement)/96-07/96109691 29 200822991 shed-shaped silk fabric has no filament and excellent resolution, and is useful for strongly bonding metal members. Preservation - [Comparative Example 1] In the Example, the composition of the paste silver particles was adjusted in the same manner as in Example 1 except that the volatile dispersion medium (10) was not added as the volatile dispersion medium (= part). Separation of silver particles with: hair = moon medium was observed in the syringe. The results are shown in Table 3. [Comparative Example 2] In Example 1, except that the μ alcohol fraction was used as The volatile dispersing medium (10) was used as a transmissive dispersing medium (Β2). The paste silver particle composition was prepared in the same manner as in Example 1. As a volatile dispersing medium (Β1), 14.8 parts of the alcohol and as a volatile matter 0.2 parts of the disperse medium (Β2) was mixed into a transparent form, and even if it was left to stand, it was not separated into two layers. The paste-like silver particle composition was observed in the syringe and the particles were dispersed. Separation of the media. The results are shown in Table 3. 1 " [Comparative Example 3] In Example 1, except that 2 parts of phenolic alcohol was used as the volatile dispersing medium (Β1) and 1·hexane was 14.8 parts. As a volatile dispersion medium (β2),
貫施例1同樣地調製糊狀銀粒子組成物。作為揮發性分散 媒（Β1)之0· 2份 > 醇以及作為揮發性分散媒（Eg)之14 g 份1 -己燒係擾拌混合變成為透明狀，即使靜置亦不會分 離為2層。该糊狀銀粒子組成物於注射器内可觀察到銀粒 子與揮發性分散媒之分離。結果整合示於表3。T 312ΧΡ/發明說明書(補件)/96-07/96109691 30 200822991 [比較例4 ] 奸於實施例1中’除了取代卜己烧而使用環己醇（和光純 藥工業股份有限公司販售之試藥，介電係數15 〇)3份作 為揮發性分散媒（B2)以外，與實施例丨同樣地調製糊狀銀 粒子組成物。作為揮發性分散媒（B1)i 12份苄醇以及作 為揮發性分散媒（B2)之3份環己醇係攪拌混合變成為透 明狀’即㈣置亦不會分離$ 2層。該肖狀銀津立子組成物 於注射器内可觀察到銀粒子與揮發性分散媒之分離。結果 整合示於表3。 ' ° [比較例5] 於實施例5中，除了取代撥水性銀粒子而使用市售之以 沈澱法製造的1次粒子平均粒徑為l 1//m(以雷射繞射法 測定）之粒狀銀粒子（未被撥水性有機物被覆，不具撥水性） 以外’與實施例5同樣地調製糊狀銀粒子組成物。該糊狀 銀粒子組成物於注射器内可觀察到銀粒子與揮發性分散 媒之分離。結果整合示於表3。 [比較例6 ] 於實施例1中，除了取代苄醇而使用乙二醇（和光純藥 工業股份有限公司販售之試藥，介電係數39· 〇)4份作為 揮叙性分散媒（B1 )、以及取代1 —己烧而使用丙酮（和光矣屯 藥工業股份有限公司販售之試藥，介電係數21 · 〇 )丨丨份作 為揮發性分散媒（B2)以外，與實施例1同樣地調製糊狀銀 粒子組成物。作為揮發性分散媒（B1)之4份乙二醇以及作 為揮發性分散媒（B2)之11份丙酮係攪拌混合變成為透明 312XP/發明說明書(補件)/96-07/96109691 31 200822991 狀即使月f置亦不會分離為2層。該糊狀銀粒 注射器内可觀察到銀粒子與揮發性分散媒敕 合示於表3。 雕、、、口禾正 [比較例7 ] ^實施例1巾’除了取_而使用乙二醇(和光純藥 工業股份有限公司販售之試藥，介電係數3 揮發性分散媒⑻）、以及取代1-己烧而使用純水（介3 數80. 0)11份作為揮發性分散媒（B2)以外，與實施例工同 樣地調製糊狀銀粒子組成物。乙二醇4份與純水U份之 混合液的介電係數為69。作為揮發性分散媒⑽之4份 乙二醇以及作為揮發性分散媒⑽之11份純水係授掉混 合變成為透明狀，即使靜置亦不會分離為2層。分散媒被 銀粒子排斥而無法成為糊狀。結果整合示於表4。、 [比較例8] 於實施例5中，除了取代撥水性銀粒子而使用市售之以 沈澱法製造的1次粒子平均粒徑為丨· 1//m(以雷射繞射法 測定）之粒狀銀粒子（未被撥水性有機物被覆，不具撥水 性），取代1,2-二乙醯氧基乙烷而使用乙二醇（和光純藥 工業股份有限公司販售之試藥，介電係數39· 〇)4份作為 揮發性分散媒（B1)、以及取代Isozol 3〇〇而使用丙_ (和 光純藥工業股份有限公司販售之試藥，介電係數21. 〇 )】工 份作為揮發性分散媒（B2)以外，與實施例5同樣地調製糊 狀銀粒子組成物。該糊狀銀粒子組成物於注射器内可觀察 到銀粒子與揮發性分散媒之分離。結果整合示於表4。 312χΡ/發明說明書(補件)/96-07/96109691 32 200822991 [比較例9] 於實施例5中，除了取代撥水性銀粒子而使用市售之以 沈殿法製造的1次粒子平均粒徑為以雷射繞射法 測定）之粒狀銀粒子（未被撥水性有機物被覆，不具撥水 性），取代1，2-二乙醯氧基乙烷而使用乙醇（和光純藥工 業股份有限公司販售之試藥，介電係數24 ())6份作為揮 發性分散媒（B1)、以及將Is〇z〇1 3〇〇之量定為9份作為 揮發性分散媒(B2)以外，與實施例5同樣地調製糊狀銀粒 子組成物。該糊狀銀粒子組成物於注射器内可觀察到銀粒 子與揮發性分散媒之分離。結果整合示於表4。 [比較例10] 於貫施例5中，除了取代撥水性銀粒子而使用市售之以 沈=法製造的1次粒子平均粒徑為i ·丨#畝以雷射繞射法 測疋）之粒狀銀粒子（未被撥水性有機物被覆，不具撥水 性）’取代1，2-二乙醯氧基乙烷而使用純水（介電係數 80· 0)6份作為揮發性分散媒（B1)、以及取代The paste silver particle composition was prepared in the same manner as in Example 1. As a volatile dispersing medium (Β1), 0.2 parts> alcohol and 14 g parts of the volatile dispersing medium (Eg) were mixed into a transparent form, and they were not separated even if they were left standing. 2 layer. The paste silver particle composition was observed to separate the silver particles from the volatile dispersion medium in the syringe. The results are shown in Table 3. T 312ΧΡ/Invention Manual (Supplement)/96-07/96109691 30 200822991 [Comparative Example 4] In Example 1, 'In addition to replacing Bucai, cyclohexanol was used (was sold by Wako Pure Chemical Industries Co., Ltd.) In the same manner as in Example 丨, a paste silver particle composition was prepared in the same manner as in Example 3, except that the volatile medium (B2) was used as the reagent. As a volatile dispersing medium (B1) i, 12 parts of benzyl alcohol and 3 parts of cyclohexanol as a volatile dispersing medium (B2) were stirred and mixed to form a transparent state, i.e., (four), and the two layers were not separated. The separation of the silver particles from the volatile dispersion medium can be observed in the syringe. Results The integration is shown in Table 3. '° [Comparative Example 5] In Example 5, except for substituting water-repellent silver particles, a commercially available primary particle having a primary particle diameter of l 1 //m (measured by a laser diffraction method) was used. In the same manner as in Example 5, the composition of the silvery silver particles was prepared in the same manner as in Example 5 except that the particulate silver particles were not coated with the water-repellent organic material. The paste silver particle composition was observed to separate the silver particles from the volatile dispersion medium in the syringe. The results are shown in Table 3. [Comparative Example 6] In Example 1, 4 parts of ethylene glycol (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant 39·〇) was used as a dissipative dispersion medium in addition to the substituted benzyl alcohol ( B1), and the substitution of 1 - burned, using acetone (a reagent sold by Wako Pharmaceutical Co., Ltd., dielectric constant 21 · 〇) as a volatile dispersion medium (B2), and examples 1 A paste silver particle composition was prepared similarly. 4 parts of ethylene glycol as the volatile dispersion medium (B1) and 11 parts of acetone as the volatile dispersion medium (B2) were stirred and mixed to become transparent 312XP/invention specification (supplement)/96-07/96109691 31 200822991 Even if the month f is set, it will not be separated into 2 layers. The silver particles and the volatile dispersion medium were observed in the paste silver particle syringe as shown in Table 3.雕,,, 口禾正 [Comparative Example 7] ^Example 1 towel 'In addition to taking _ use of ethylene glycol (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant 3 volatile dispersion medium (8)) The paste silver particle composition was prepared in the same manner as in the example except that 11 parts of pure water (3:80) was used as the volatile dispersion medium (B2) instead of the 1-hexane. The mixture of 4 parts of ethylene glycol and U of pure water had a dielectric constant of 69. 4 parts of ethylene glycol as the volatile dispersion medium (10) and 11 parts of pure water as the volatile dispersion medium (10) were mixed and changed to be transparent, and were not separated into two layers even when left standing. The dispersion medium is repelled by the silver particles and cannot be paste-like. The results are shown in Table 4. [Comparative Example 8] In Example 5, in addition to the water-repellent silver particles, a commercially available primary particle having a primary particle diameter of 丨·1//m (measured by a laser diffraction method) was used. Granular silver particles (not coated with water-repellent organic matter, not water-repellent), and substituted for 1,2-diethoxymethoxyethane, using ethylene glycol (a reagent sold by Wako Pure Chemical Industries Co., Ltd. 4 parts of electric coefficient 39·〇) as volatile dispersing medium (B1), and using instead of Isozol 3〇〇, _ (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric coefficient 21. 〇) A paste silver particle composition was prepared in the same manner as in Example 5 except that the volatile dispersion medium (B2) was used. The paste silver particle composition was observed to separate the silver particles from the volatile dispersion medium in the syringe. The results are shown in Table 4. 312χΡ/发明发明(补件)/96-07/96109691 32 200822991 [Comparative Example 9] In Example 5, except for substituting water-repellent silver particles, a commercially available primary particle diameter of the primary particle method was Granular silver particles (measured by laser diffraction method) (not water-repellent organic coated, not water-repellent), replacing ethanol with 1,2-diethoxymethoxyethane (Wako Pure Chemical Industries Co., Ltd.) For the test drug, the dielectric constant of 24 ()) is 6 parts as the volatile dispersion medium (B1), and the amount of Is〇z〇1 3〇〇 is set to 9 parts as the volatile dispersion medium (B2). In the fifth embodiment, a paste silver particle composition was prepared in the same manner. The paste silver particle composition was observed to separate the silver particles from the volatile dispersion medium in the syringe. The results are shown in Table 4. [Comparative Example 10] In Example 5, except for substituting the water-repellent silver particles, a commercially available one-particle average particle diameter manufactured by the sinking method was i · 丨 # mu measured by a laser diffraction method) Granular silver particles (not coated with water-repellent organic matter, not water-repellent) 'substituted 1 ,2-diethoxymethoxyethane and 6 parts of pure water (dielectric coefficient 80·0) as volatile dispersion medium ( B1), and replace
Isozol 300 而使用乙醇（和光純藥工業股份有限公司販售之試藥，介 電係數24.0)9份作為揮發性分散媒（β2)以外，與實施例 5同樣地凋衣糊狀銀粒子組成物。純水6份與乙醇9份之 此口液的介電係數為46 4。該糊狀銀粒子組成物於注射 裔内可觀察到銀粒子與揮發性分散媒之分離。結果整合示 於表4。 [比較例11] 於貝加例7中，除了取代乙二醇而使用純水（介電係數 312XP/發明說明書(補件)/96·〇7/96ΐ〇9691 33 200822991 80· 0)15份作為揮發性分散媒以外，與實施例7同樣地調 製糊狀銀粒子組成物。揮發性分散媒被銀粒子排斥而無法 成為糊狀。結果整合示於表4。 … [比較例12] 於κ %例7中，除了取代乙二醇而使用is〇z〇i 3〇〇(新 日本石油股份有限公司販f之異錢混合物，介電係數 份作為揮發性分散媒以外，與實施例7同樣地調 製糊狀銀粒子組成物。該糊狀銀粒子組成物於注射器内可 親察到銀粒子與揮發性分散媒之分離。結果整合示於表4。 [比較例13] 於實施例7中，降了 & r ^ ^ 除了取代乙二醇而使用卜辛醇（和光純 ^工業股份有限公司販售之試藥，介電係數旧加份作 f:發性分散媒以外，與實施例7同樣地調製糊狀銀粒子 :捏：ηΛ:狀銀粒子組成物於注射器内可觀察到銀粒子 刀散媒之分離。結果整合示於表 [比較例14] (以對乂〇〇二之市售之以沈澱法製造、1次粒子的平均粒徑 (以雷射繞射法測定）為1】ϊ 仪 性有機物«，不㈣水性），2絲狀絲子（未被撥水 為Ί售之試藥，介電係數31.〇)作 糊狀使用旋轉式混練機均勾混合，調製 發粒Γ组成物於注射器内可觀察到銀粒子與揮 I性分散媒之分離。結果整合示於表5。 3咖/發明說明書(補件)/9嶋61咖 34 200822991 [比較例15 ] r對100份之市售之以沈殺法製造、1次粒子的平均師 (以雷射繞射法測定)為u㈣之粒狀銀粒子(未被撥水 =機物被覆，不具撥水性），添加75份之丙⑼ 屯樂工業股份有限公司販售之，介電係數3u)作ί 揮發性分散媒（C)，使用旋轉式混缴 … 狀銀粒子組成物。 相均“合，調製糊 义該糊狀銀粒子組成物於注射器内可觀察㈣粒子與揮 赉性分散媒之分離。結果整合示於表5。 [比較例16] 對_份之市售之以輯法製造、丨次粒子 (以雷射繞射法測定）為1 1 " m ^ ^ M ± m Ain U m · 之粒狀銀粒子（未被撥水 w ^ ，、概以生），添加75份之乙二醇（和光 »、、屯藥工業股份有限公司販售 人雨/ 揮發性分散媒（«，使^轉\：?_介^係數39.0)作為 狀銀粒子組成物。 “練機均勻混合，調製糊 ^ 糊狀銀粒子組成物於注射器内可觀察到銀粒子與揮 ^ f生为散媒之分離。結果整合示於表5。 [比較例17] ' 對10 0份之市售之以沈：殿土每】 (以雷射繞射法測定：/；!1次粒子的平均粒徑 =機勿被覆，不具撥水性），添加75份之純水（蒸 二電係數80.0)作為揮發性分散媒⑽、75份之14_丁 -知（和光純藥工業股份有限公司販售之試藥，介電係數 M2XP/發明說明書(補件)/96-07/96109691 35 200822991 3U)作為揮發性分散媒⑽、以及& 75份之 純藥工業股份有限公司販售之試藥，介電係數2 ^ 揮發性分散媒（B2)，使用旋轉式混練機均句混人 : 狀銀粒子組成物。 〇调製糊 :糊狀銀粒子組成物於注射器内可觀察到 發性分散媒之分離。結果整合示於表6。 /、禪 [比較例18 ] 對100份之市售之以沈澱法製造、卜欠 2有機物被覆，不具撥水性），添加75份之純 介電係數80.0)作為揮發性分散媒（B1)、75份之、、丙^醇 屯藥工業股份有限公司販售之試藥，介電係數 作為揮發性分散媒（B2)、以及3 7 · 蚩η凡々、士 \ · 75知之丙酮（和光純藥工 司販售之試藥，介電係數2ΐ·(υ作為揮發性 二、=二)，使用旋轉式混練機均勻混合，調製糊狀銀粒 :糊狀銀粒子組成物於注射器内可觀察到銀粒子與揮 叙性力放媒之分離。結果整合示於表6。 [比較例19] 卜^100伤之市售之以沈殿法製造、1次粒子的平均粒徑 (以雷射繞射法測定）為彳7 性有嬙你u 、、、· U 10之粒狀銀粒子（未被撥水 介，不具撥水性），添加75份之純水（蒸餾水， 二:.〇)作為分散媒（揮發性分散媒（B1))、75份之 一醇（和光純藥工業股份有限公司販售之試藥，介電係 312XP/發明說明書(補件)/96-07/96109691 ^ 36 200822991 數39. 0 )作為揮發性分散媒（B2)、以及3· 75份之丙酮（和 光純藥工業股份有限公司販售之試藥，介電係數21.0)作 為揮發性分散媒（Β2)，使用旋轉式混練機均勻混合，調製 糊狀銀粒子組成物。 該糊狀銀粒子組成物於注射器内可觀察到銀粒子與揮 發性分散媒之分離。結果整合示於表6。 312ΧΡ/發明說明書(補件)/96-07/96109691 37 200822991[表1]In the case of Isozol 300, 9 parts of ethanol (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant 24.0) was used as a volatile dispersion medium (β2), and a paste-like silver particle composition was obtained in the same manner as in Example 5. . The dielectric constant of 6 parts of pure water and 9 parts of ethanol was 46 4 . The paste silver particle composition was observed to separate the silver particles from the volatile dispersion medium in the injection. The results are shown in Table 4. [Comparative Example 11] In Baye's Example 7, pure water (dielectric coefficient 312XP/invention specification (supplement)/96·〇7/96ΐ〇9691 33 200822991 80·0) was used in place of ethylene glycol. A paste silver particle composition was prepared in the same manner as in Example 7 except for the volatile dispersion medium. The volatile dispersion medium is repelled by the silver particles and cannot be paste-like. The results are shown in Table 4. [Comparative Example 12] In κ % Example 7, except for the substitution of ethylene glycol, is〇z〇i 3〇〇 (New Japan Petroleum Co., Ltd.) In the same manner as in Example 7, a paste silver particle composition was prepared in the same manner as in Example 7. The paste silver particle composition was observed in the syringe to separate the silver particles from the volatile dispersion medium. The results are shown in Table 4. Example 13] In Example 7, the reduction & r ^ ^ was used in addition to the ethylene glycol, and the use of the octanol (a reagent sold by Wako Pure Chemical Industries Co., Ltd., the old dielectric constant for f: hair In the same manner as in Example 7, the paste silver particles were prepared in the same manner as in Example 7 except that the silver particles were separated from the syringe by the kneading: ηΛ: silver particle composition. The results are shown in the table [Comparative Example 14]. (Improved by the precipitation method, the average particle size of the primary particles (measured by the laser diffraction method) is 1] 仪 organic matter «, not (four) water), 2 filamentous Sub-subject (testing drug that has not been dialed for sale, dielectric constant 31. 〇) as a paste using rotary kneading machine The mixture of the granules and the composition of the granules was observed in the syringe to observe the separation of the silver particles from the volatile dispersion medium. The results are shown in Table 5. 3 Coffee/Invention Manual (Supplement)/9嶋61 Coffee 34 200822991 [ Comparative Example 15] r to 100 parts of commercially available granular silver particles (manufactured by laser diffraction method) which were manufactured by the method of sinking, and which were not water-repellent = machine-coated, No water repellency), adding 75 parts of C (9) sold by 屯乐工业股份有限公司, dielectric constant 3u) for ί volatile dispersion media (C), using a rotating mixture of... silver particles composition. "Combination, preparation of the paste silver particle composition can be observed in the syringe (4) separation of the particles from the volatile dispersion medium. The results are shown in Table 5. [Comparative Example 16] Method of manufacturing, 丨 sub-particles (measured by laser diffraction method) is 1 1 " m ^ ^ M ± m Ain U m · granular silver particles (not watered w ^ , all in life), added 75 parts of ethylene glycol (Heguang »,, Peony Pharmaceutical Co., Ltd. sells human rain / volatile dispersion media («, make ^ turn \:?_介^ coefficient 39 .0) As a composition of silver particles. "Mixed evenly, the paste is prepared. The composition of the paste silver particles can be observed in the syringe. The separation of the silver particles from the silver particles is observed. The results are shown in Table 5. [Comparative Example 17] 'For the 10 parts of the market, Shen: Dianmu every】 (Measured by laser diffraction method: /;! The average particle size of the first-order particles = machine is not covered, no water-repellent) , adding 75 parts of pure water (steamed two electric coefficient 80.0) as a volatile dispersing medium (10), 75 parts of 14_Ding-zhi (a reagent sold by Wako Pure Chemical Industries Co., Ltd., dielectric constant M2XP / invention manual (Supplement)/96-07/96109691 35 200822991 3U) As a volatile dispersing medium (10), and & 75 parts of the pure drug industry limited company sold, the dielectric coefficient 2 ^ volatile dispersion medium (B2 ), using a rotary kneading machine to mix people: silver particles composition. 〇 Modulation paste: The composition of the paste-like silver particles can be observed in the syringe. The results are shown in Table 6. /, Zen [Comparative Example 18] For 100 parts of the commercially available method of precipitation, 2 organic coatings, no water repellency, adding 75 parts of pure dielectric constant 80.0) as volatile dispersion medium (B1), 75 parts of the reagents sold by propylene phenolic pharmaceutics co., Ltd., the dielectric constant is used as the volatile dispersing medium (B2), and 3 7 · 蚩 々 々 々 士 士 士 \ \ 丙酮 ( The reagents sold by the company, the dielectric constant is 2ΐ·(υ as volatility II, =2), and evenly mixed using a rotary kneading machine to prepare paste silver particles: the composition of the paste silver particles can be observed in the syringe. The separation of the silver particles and the dissipative force media. The results are shown in Table 6. [Comparative Example 19] The product of the Bu-100 injury is commercially available in the Shen Dian method, and the average particle size of the primary particles (with laser diffraction) Method for the determination of 彳7 嫱 u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u u Medium (volatile dispersion medium (B1)), 75 parts of one alcohol (tested by Wako Pure Chemical Industries Co., Ltd., dielectric system 31 2XP/Inventive Manual (Repair)/96-07/96109691 ^ 36 200822991 No. 39. 0 ) As volatile dispersion medium (B2), and 3.75 parts of acetone (Wako Pure Chemical Industries Co., Ltd. sold for sale) Drug, dielectric constant 21.0) as a volatile dispersing medium (Β2), uniformly mixed using a rotary kneader to prepare a paste silver particle composition. The paste silver particle composition can be observed in the syringe with silver particles and volatility The separation of the dispersion media. The results are shown in Table 6. 312ΧΡ/Invention Manual (supplement)/96-07/96109691 37 200822991 [Table 1]
金屬粒子 [形狀/平均粒徑] 調配量 子 (還原法) [碎片狀 /3.0/zm] 100份 銅粒子 [碎片狀 /4.0/zin] 100份 鎳粒子 [碎片狀 /6.0//m] 100份 練子 餘子 (還原法） [碎片狀 /3.0/zm] 100份 [粒；yt/l· 1/ζιη] 100份 [粒JR/1· l"m] 100份Metal particles [shape/average particle size] Blending quantum (reduction method) [Fragmentation/3.0/zm] 100 parts of copper particles [fragmentation/4.0/zin] 100 parts of nickel particles [fragmentation/6.0//m] 100 parts Practicing the remainder (reduction method) [Fragmentation/3.0/zm] 100 parts [grain; yt/l·1/ζιη] 100 parts [grain JR/1·l"m] 100 parts
揮發f生分散媒(B1) (介電係數） 調配量 苄醇 (介電係數 13.0) 12份 苄醇 (介電係數 13.0) 12份 雙(2-乙氧基乙 基)醚 (介電係數5.6) 11份 (介電係數 38.0) 12份 1,2-二乙醯氧基乙烷 (介電係數7.3) 14份 甲基正己基嗣 (介電係數12.2) 14份 揮發I*生錄媒(B2) (介電係數） 調配量 (Bl) : (B2) (B1)與(B2)之相激生 金屬粒子瓣雜分散 媒之分離性(刪） 黏著強度A(kgf) 黏著強度B(kgf) [表2] 1-己燒 (介電係數 2.0) 3份 12： 2層分離 24 1-己烷 (介電係數 2.0) 3份 12:3 2層分離 1-己烷 (介電係數 2.0) 3份 12:3 2層分離 乙二醇 (介電係數 39.0) __4# 11 2層分離Volatile f-dispersion medium (B1) (dielectric coefficient) Formulation amount of benzyl alcohol (dielectric coefficient 13.0) 12 parts of benzyl alcohol (dielectric coefficient 13.0) 12 parts of bis(2-ethoxyethyl)ether (dielectric coefficient) 5.6) 11 parts (dielectric coefficient 38.0) 12 parts of 1,2-diethoxymethoxyethane (dielectric coefficient 7.3) 14 parts of methyl-n-hexyl hydrazine (dielectric coefficient 12.2) 14 parts of volatile I* bio-recording medium ( B2) (Dielectric coefficient) Blending amount (Bl): (B2) Separation of the excited metal particle bulk dispersing medium between (B1) and (B2) (deletion) Adhesive strength A (kgf) Adhesive strength B (kgf [Table 2] 1-hexane (dielectric coefficient 2.0) 3 parts 12: 2 layers separation 24 1-hexane (dielectric coefficient 2.0) 3 parts 12:3 2-layer separation 1-hexane (dielectric coefficient 2.0 3 parts 12:3 2 layers of separated ethylene glycol (dielectric coefficient 39.0) __4# 11 2 layers separation
Isozol 300 (異石蠟混合物，介t|( 係數2.1) _2份 純水 丨蒸顧水，介電係 數 80.0) 2份 14:2 2層分離 14:2 2層分離 實施例7 實施例8 實施例9 實施例10 實施例11 金屬粒子 [形似平均粒徑] 調配量 #^立子 (還原法） [碎片狀 /3.0//ra] 100份 銅粒子 [碎片狀 /4.0/zm] 100份 鎳粒子 [碎片狀 /6.0/zm] 100份 船立子 (舰法） [粒狀/Ι.ίμιη] 100份 ^^立子 (還原法） [碎片狀/3.0/zm] 100份 被覆劑 (重量％) 硬脂酸 (0.5重量％) 娜旨酸 (0.5重量％) 油酸 (0.8重量％) 硬脂酸 (1.5重量％) 硬脂酸 (〇·5重量 揮雜分散媒(B1)或(C) (介電係數） 調配量 乙二醇 (介電係數 39.0) 15份 甘油 (介電係數 47.0) 15份 甘油 (介電係數 47.0) 15份 Ν,Ν-二甲基甲醯 胺 (介電係數38.0) 15份 純水 (蒸顧水，介電係數 80.0) 15份 揮雜錄媒(B2) (介電係數） 調配量 — — — 一 乙醇 (介電係數24.0) 3份 (ΒΠ ： (B2) — — 一 — 15:3 (B1)與(B2)之相溶性 — — — 一 未分離 金屬粒子與揮發ϋ分散媒之分離 性(刪） 0 0 0 0 0 黏著強度A(kgf) 14 — 一 17 12 黏著強度B(kgf) — — — — — 312XP/發明說明書(補件)/96-07/96109691 38 200822991 [表3] 比較例1 比較例2 比較例F —比較例4 π 金屬粒子 [形狀/平均粒徑] 調配量 2上西女.1 錄子 (還原法） [碎片狀 /3. O^m] 100份 錄子 (還原法） [碎片狀 /3.0"m] 100份 子 (還原法） [碎片狀 /3. O^m] 100份 雜子 (還原法） [碎片狀 /3.0"m] 100份 比竿又 1 夕1J ί) 雜子 (舰去） [粒狀 100份 —味例6 錄子 (還原法） [碎片狀 /3· 0卵] 被覆劑 一（重量％) 硬脂酸 (〇. 5重量％) 硬脂酸 (0.5重量％) 硬脂酸 (〇. 5重量 硬脂酸 (0.5重量％、 無 100份 硬脂酸 揮發1*生分散媒(B1) (介電係數） 調配量 苄醇 (介電係數 13.0) 15份 苄醇 (介電係數 13.0) 14· 8 份 苄醇 (介電係數 13.0) 0,2份 苄醇 (介電係數 13.0) 12份 ---— 1，2-二乙醯氧基乙烷 (介電係數7.3) 14份 (0.5重量 乙二醇 (介電係數 39· 0) 揮雜錄媒(B2) (介電係數） 調西己量 —_ (Bl) ： (B2) 一 1-己烧 (介電係數 2.0) 0.2份 14. R ： Π 9 1-己烷 (介電係數 2.0) 14.8 份 (\ 〇 · Λλ Q 環己醇 (介電係數 15.0) 3份 Isozol 300 (異石蝶混錄，介電係 數 2.1) — 2份 ,4份 丙酮 (介電係數 21.0) 11份 (B1)與(B2)之相溶性 未分離 丄4*· 〇 · U·乙 未分離 U. ώ · 14. 〇 未分離 12 : 3 未分離 14:2 2層分離 4:11 来分離 金屬粒子與揮雜分散媒 之分離性(腿） 黏著強度(krf) 2.0 2.0 3.0 2.5 ----- 1.5 **vF· 1.0 4 [表4] 金屬粒子 [形狀/平均粒徑] 調配量 比較例7 ^^立子 (細去） [碎片狀/3.0卵] 100份 比較例8 絲子 [粒狀 /1. l//m] 100份 比較例9 立子 [粒狀/1· l//m] 100份 比較例10 ^^立子 (舰法） [粒似1· 1仰: 100份 —比較例11 立子 (還原法） [碎片狀/3.0/zm] 100份 _ 比較例12 錄子 (還原法） [碎片狀/3.0/zm] 100份 被覆劑 (金屬粒子中之撥冰 有機物量，重量 %) . 硬脂酸 (〇·5重量％) 無 無 無 i—— - 硬脂酸 (〇· 5重量％) 魏酸 (0.5重量％) 揮概分散媒(B1) 乙二醇 (介電係數39.0) 4份 乙二醇 (介電係數 39.0) 4份 乙醇 (介電係數24.0) 6份 純水 (蒸館水，介電 係數80_0) 6份 脉 (蒸館水，介電係_ 80.0) 15价 Isozol 300 (異石蠟混射勿， 介電係數2.1) 揮姐錄媒(B2) 純水 (蒸館水，介電係數 80.0) —11份 丙酮 (介電係數 21.0) 11份 Isozol 300 (異石蝶混娣， 介電係數2.1) 9份 乙醇 (介電係數 24.0) 9份 15份 禪刺生昆 合比率(B1) ·· ίΒ2) 4^2欠·LiL八从/ 1从1 4:11 4:11 6:9 6:9 — 揮發14：^:媒之相 溶性 未分離 未分離 未分離 未分離 未分離 未分離 金屬粒子與揮發('生 綠媒之分離性 (ram) 黏著強度(krf) 錄媒雜粒子排 斥而無法成為糊狀 2.0 5 2.0 3.0 錄媒琴紙粒子排 斥而無法成為糊狀 3.0 39 312χρ/發明說明書(補件)/96-07/96109691 200822991 [表5] 比較例13 嘯列14 比較例15 交例16 金屬粒子 綠子 ^#立子 錄子 ^ 11^-4 X w ^#立子 [形似平均粒徑] (還原法） (細έ) ⑻敝） 調配量 [碎片狀/3_0/im] [粒似1· 1 /zm] [粒狀/1.1 //in] [粒狀/1· l"m] 100份 100份 100份 100份 被覆劑 (金屬粒子中之撥水性有機物量，重量％) 硬脂酸 (0.5重量％) 無 無 無 揮發分散媒(B1)或(C) 1-辛醇 1,4-丁二8| 丙二Si 乙二醇 (介電係數10.0) (介電係數31.0) (介電係數34.0) (介電係數39· 0) 15份 75份 75份 75份 —— 揮發f生綠媒(B2) — 一 揮發〖生分散媒之混合比率(Bl) : (B2) — 一 _ 未分離 未分離 未分離 未分離 金屬粒子鄉槪綠媒之分離性(腿） 2.0 6.0 6.0 7.0 黏著強度(kgf) — 嚴重分離而無法測定 嚴重分離而無法測定 嚴重分離而無法：測定 [表6] 比較例17 比較例18 比較例19 金屬粒子 [形似平均粒徑] 調配量 子 (舰έ) [粒似1· 1 "m] 100份 雜子 (舰去） [粒飢1/ai] 100份 錄子 (光餘） [粒 JR/1.1/zm] 100份 被覆劑 _(金屬粒子中之撥水性有機物詈，重詈 無 無 無 揮紐纖某(B1) 脉 (蒸德水，介電係數80.0) 75份 純水 (蒸德水，介電係數80.0) 75份 脉 (蒸館水，介電係數80, 〇) 75份 揮雜錄媒(B2) 1,4 -丁二醇 (介電係數31.0) 75份 丙二# (介電係數34.0) 75份 乙二醇 (介電係數39.0) 75份 揮發f生錄媒(B2) 丙酮 (介電係數21.0) 3.75 份 丙嗣 (介電係數21.0) 3.75 份 丙酮 (介電係數21.0) 3 75价 揮發1*生分散媒之混合比率(Bl) : (B2) : (B2) 75： 75： 3.75 75 : 75 : 3.75 75 ： 75 ： 3.7R ~ 揮發f生^:媒:^目溶性 未分離 未分離 未分離 金屬粒子絲雜練媒之分離性(腿） 14.0 15.0 15.0 黏著強度(tef) 嚴重分離而無法測定 嚴重分離而無法測定 嚴重分離而無法測定 40 312ΧΡ/發明說明書(補件)/96-07/96109691 200822991 (產業上之可利用性） 本發明之糊狀金屬粒子組成物， 計算單 金屬粒子與揮發性分散叙分離，仍不會發生 於金屬製構件的黏合方面係有用的 ^性優異，因此 之黏合方法在將電容器、電阻、二極體明之金屬製構件 等晶片零件黏合到基板方面係有記^ 【圖式簡單說明】 ’用的。 離性的 圖1係實施例中金屬粒子與揮 測定之注射器的侧面圖。 ^生刀散媒之分 【主要元件符號說明】 Α 分離性試驗器 1 糊狀金屬粒子組成物 2 前端蓋 3 注射器 4 活塞 5 尾端蓋 312ΧΡ/發明說明書(補件)/96-07/96109691 41Isozol 300 (isoparaffin mixture, t = (factor 2.1) _2 parts pure water, steamed water, dielectric coefficient 80.0) 2 parts 14:2 2 layers separation 14: 2 2 layers separation Example 7 Example 8 Example 9 Example 10 Example 11 Metal particles [Shape-like average particle diameter] Formulation amount #^立子(Reduction method) [Fragmentation/3.0//ra] 100 parts of copper particles [fragmentation/4.0/zm] 100 parts of nickel particles [ Fragmentation / 6.0/zm] 100 parts of the ship (ship method) [granular / Ι. ίμιη] 100 parts ^ ^ stand (reduction method) [fragmentation / 3.0 / zm] 100 parts of coating (% by weight) stearin Acid (0.5% by weight) Natto acid (0.5% by weight) Oleic acid (0.8% by weight) Stearic acid (1.5% by weight) Stearic acid (〇·5 weight of volatile dispersion medium (B1) or (C) Electric coefficient) Formulation amount of ethylene glycol (dielectric coefficient 39.0) 15 parts of glycerin (dielectric coefficient 47.0) 15 parts of glycerol (dielectric coefficient 47.0) 15 parts of hydrazine, hydrazine-dimethylformamide (dielectric coefficient 38.0) 15 parts pure water (distilled water, dielectric coefficient 80.0) 15 parts of mixed media (B2) (dielectric coefficient) dosage - - one ethanol (dielectric coefficient 24.0) 3 parts (ΒΠ: (B2) - — 一 — 15:3 (B1) and (B2) Compatibility - Separation of an unseparated metal particle from a volatile oxime dispersing medium (deleted) 0 0 0 0 0 Adhesion strength A (kgf) 14 - a 17 12 Adhesion strength B (kgf) — — — — — 312XP/ Inventive specification (supplement)/96-07/96109691 38 200822991 [Table 3] Comparative Example 1 Comparative Example 2 Comparative Example F - Comparative Example 4 π Metal particles [Shape / Average Particle Diameter] Preparation amount 2 Upper Western female. 1 Record Sub-reduction method [fragmentation / 3. O^m] 100 parts (reduction method) [fragmentation / 3.0 " m] 100 parts (reduction method) [fragmentation / 3. O^m] 100 parts Miscellaneous (reduction method) [Fragmentation / 3.0 " m] 100 copies 竿 1 1 1J ί) Miscellaneous (ship to go) [100 pieces of granularity - taste example 6 recording (reduction method) [fragmentation / 3·0 eggs] coating agent one (% by weight) stearic acid (〇. 5 wt%) stearic acid (0.5% by weight) stearic acid (〇. 5 weights of stearic acid (0.5% by weight, no 100 parts hard) Fatty acid volatilization 1* Raw dispersion medium (B1) (Dielectric coefficient) Formulation amount of benzyl alcohol (dielectric coefficient 13.0) 15 parts of benzyl alcohol (dielectric coefficient 13.0) 14·8 parts of benzyl alcohol (dielectric coefficient 13.0) 0, 2 parts of benzyl alcohol (dielectric coefficient 13.0) 12 Parts---- 1,2-diethoxymethoxyethane (dielectric coefficient 7.3) 14 parts (0.5 weight ethylene glycol (dielectric coefficient 39·0) volatile media (B2) (dielectric coefficient)调西己量—_ (Bl) : (B2) 1-1-burn (dielectric coefficient 2.0) 0.2 parts 14. R : Π 9 1-hexane (dielectric coefficient 2.0) 14.8 parts (\ 〇· Λλ Q Cyclohexanol (dielectric coefficient 15.0) 3 parts Isozol 300 (mixed stone butterfly, dielectric constant 2.1) - 2 parts, 4 parts acetone (dielectric coefficient 21.0) 11 parts (B1) and (B2) compatibility Unseparated 丄4*· 〇· U·B not separated U. ώ · 14. 〇 not separated 12 : 3 unseparated 14:2 2 layers separated 4:11 to separate the separation of metal particles from the dispersing medium (legs) Adhesion strength (krf) 2.0 2.0 3.0 2.5 ----- 1.5 **vF· 1.0 4 [Table 4] Metal particles [shape/average particle size] Comparative amount comparison example 7 ^^立子(细去) [Fragmentation/ 3.0 eggs] 100 parts Comparative Example 8 Silk [granular / 1. l / / m] 100 parts of Comparative Example 9 Lizi [granular / 1 · l / / m] 100 parts of Comparative Example 10 ^ ^ Lizi (ship method) [Grain like 1·1 elevation: 100 parts - Comparative Example 11 Lizi (reduction method) [Fragmentation/3.0/zm] 100 parts _ Comparative Example 12 Recorder ( Original method) [Fragmentation/3.0/zm] 100 parts of coating agent (amount of iced organic matter in metal particles, % by weight). Stearic acid (〇·5 wt%) No or no i——- Stearic acid ( 〇·5 wt%) Wei acid (0.5% by weight) Dispersing medium (B1) Ethylene glycol (dielectric coefficient 39.0) 4 parts ethylene glycol (dielectric coefficient 39.0) 4 parts ethanol (dielectric coefficient 24.0) 6 Pure water (steamed water, dielectric coefficient 80_0) 6 veins (steamed water, dielectric _ 80.0) 15 price Isozol 300 (isoparaffin mixed, dielectric coefficient 2.1) Sister media (B2) Pure water (steamed water, dielectric coefficient 80.0) - 11 parts of acetone (dielectric coefficient 21.0) 11 parts of Isozol 300 (isolithic butterfly mixed, dielectric constant 2.1) 9 parts of ethanol (dielectric coefficient 24.0) 9 parts 15 The ratio of Zen thorns to stagnation (B1) ·· ίΒ2) 4^2 owe · LiL eight from / 1 from 1 4:11 4:11 6:9 6:9 — Volatilization 14:^: The compatibility of the media is not separated Unseparated, unseparated, unseparated, unseparated, unseparated metal particles and volatilized (separation of morbidity (ram) adhesion strength (krf) recording medium particle repulsion and cannot be pasty 2.0 5 2.0 3.0 recording media paper particle exclusion Can't be Shape 3.0 39 312 χ ρ / invention manual (supplement) / 96-07/96109691 200822991 [Table 5] Comparative Example 13 Xiao Er 14 Comparative Example 15 Example 16 Metal particle green child ^ #立子录子 ^ 11^-4 X w ^#立子[Like average particle size] (Reduction method) (fine έ) (8) 敝) The amount of preparation [fragmentation / 3_0 / im] [grain like 1 · 1 / zm] [granular / 1.1 / in] [grain Shape/1·l"m] 100 parts 100 parts 100 parts 100 parts of coating agent (amount of water-repellent organic matter in metal particles, weight%) Stearic acid (0.5% by weight) No non-volatile dispersion medium (B1) or C) 1-octanol 1,4-butane 8 | propylene di-Si ethylene glycol (dielectric coefficient 10.0) (dielectric coefficient 31.0) (dielectric coefficient 34.0) (dielectric coefficient 39 · 0) 15 parts 75 parts 75 parts of 75 parts - volatile f green medium (B2) - a volatile mixture ratio of raw media (Bl): (B2) - a _ unseparated, unseparated, unseparated, unseparated metal particles, nostalgic green media separation Sex (leg) 2.0 6.0 6.0 7.0 Adhesion strength (kgf) - severe separation and inability to measure severe separation and inability to measure severe separation cannot be determined: [Table 6] Comparative Example 17 Comparative Example 18 Comparative Example 19 Metal particles [Like Average particle size] Blending quantum (ship) [granules like 1·1 "m] 100 miscellaneous (ship to go) [grain hunger 1 / ai] 100 copies (light surplus) [grain JR/1.1/zm ] 100 parts of coating agent _ (the water-repellent organic matter in the metal particles, 詈 詈 无 无 无 无 无 (B1) pulse (steamed water, dielectric coefficient 80.0) 75 parts of pure water (steamed water, dielectric Coefficient 80.0) 75 parts pulse (steamed water, dielectric coefficient 80, 〇) 75 parts of mixed media (B2) 1,4-butanediol (dielectric coefficient 31.0) 75 parts of propylene 2 (dielectric coefficient 34.0 75 parts of ethylene glycol (dielectric coefficient 39.0) 75 parts of volatile f-recording medium (B2) acetone (dielectric coefficient 21.0) 3.75 parts of propylene (dielectric coefficient 21.0) 3.75 parts of acetone (dielectric coefficient 21.0) 3 75 Valence volatilization 1* Mixing ratio of raw dispersion medium (Bl) : (B2) : (B2) 75: 75: 3.75 75 : 75 : 3.75 75 : 75 : 3.7R ~ Volatilization f Raw ^: Medium: ^ Eye solubility is not separated Separation of unseparated unseparated metal particle silk scouring media (legs) 14.0 15.0 15.0 Adhesion strength (tef) Severe separation and inability to measure severe separation and inability to measure severe separation cannot be determined 40 312 ΧΡ / Invention specification (supplement) / 96 -07/96109691 20082 2991 (Industrial Applicability) The paste-like metal particle composition of the present invention is obtained by calculating the separation of the single metal particles from the volatile dispersion, and is still excellent in the adhesion of the metal member. The bonding method is used to bond a wafer component such as a capacitor, a resistor, or a metal member such as a diode to a substrate. Displacement Figure 1 is a side view of a metal particle and a syringe for the measurement in the examples. ^The raw material of the knife [Description of the main components] Α Separation tester 1 Paste metal particle composition 2 Front end cover 3 Syringe 4 Piston 5 End cap 312 ΧΡ / invention manual (supplement) /96-07/96109691 41