TWI819082B - 銀奈米粒子、導電性接著劑、燒結體、及構件間具備燒結體的裝置 - Google Patents
銀奈米粒子、導電性接著劑、燒結體、及構件間具備燒結體的裝置 Download PDFInfo
- Publication number
- TWI819082B TWI819082B TW108131529A TW108131529A TWI819082B TW I819082 B TWI819082 B TW I819082B TW 108131529 A TW108131529 A TW 108131529A TW 108131529 A TW108131529 A TW 108131529A TW I819082 B TWI819082 B TW I819082B
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- Taiwan
- Prior art keywords
- silver nanoparticles
- sintered body
- silver
- conductive adhesive
- acid
- Prior art date
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 239000000853 adhesive Substances 0.000 title claims description 51
- 230000001070 adhesive effect Effects 0.000 title claims description 49
- 239000002245 particle Substances 0.000 claims abstract description 65
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052709 silver Inorganic materials 0.000 claims abstract description 30
- 239000004332 silver Substances 0.000 claims abstract description 30
- 238000004455 differential thermal analysis Methods 0.000 claims abstract description 22
- 239000002105 nanoparticle Substances 0.000 claims abstract description 15
- 239000013585 weight reducing agent Substances 0.000 claims abstract description 9
- -1 amine compound Chemical class 0.000 claims description 46
- 239000002904 solvent Substances 0.000 claims description 25
- 238000005259 measurement Methods 0.000 claims description 12
- 238000005304 joining Methods 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 33
- 239000000203 mixture Substances 0.000 description 32
- 235000014113 dietary fatty acids Nutrition 0.000 description 25
- 229930195729 fatty acid Natural products 0.000 description 25
- 239000000194 fatty acid Substances 0.000 description 25
- 150000004665 fatty acids Chemical class 0.000 description 13
- 238000010438 heat treatment Methods 0.000 description 13
- 238000003756 stirring Methods 0.000 description 13
- 238000000034 method Methods 0.000 description 12
- 238000005245 sintering Methods 0.000 description 12
- 239000011248 coating agent Substances 0.000 description 11
- 238000000576 coating method Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 10
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- 239000003495 polar organic solvent Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 239000007788 liquid Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 7
- 238000004458 analytical method Methods 0.000 description 7
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- 150000001298 alcohols Chemical class 0.000 description 6
- 125000004432 carbon atom Chemical group C* 0.000 description 6
- PAFZNILMFXTMIY-UHFFFAOYSA-N cyclohexylamine Chemical compound NC1CCCCC1 PAFZNILMFXTMIY-UHFFFAOYSA-N 0.000 description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 6
- DPBLXKKOBLCELK-UHFFFAOYSA-N pentan-1-amine Chemical compound CCCCCN DPBLXKKOBLCELK-UHFFFAOYSA-N 0.000 description 6
- 230000000704 physical effect Effects 0.000 description 6
- XNGYKPINNDWGGF-UHFFFAOYSA-L silver oxalate Chemical compound [Ag+].[Ag+].[O-]C(=O)C([O-])=O XNGYKPINNDWGGF-UHFFFAOYSA-L 0.000 description 6
- 239000006228 supernatant Substances 0.000 description 6
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- BMVXCPBXGZKUPN-UHFFFAOYSA-N 1-hexanamine Chemical compound CCCCCCN BMVXCPBXGZKUPN-UHFFFAOYSA-N 0.000 description 5
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- 238000003760 magnetic stirring Methods 0.000 description 5
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- ULQISTXYYBZJSJ-UHFFFAOYSA-N 12-hydroxyoctadecanoic acid Chemical compound CCCCCCC(O)CCCCCCCCCCC(O)=O ULQISTXYYBZJSJ-UHFFFAOYSA-N 0.000 description 4
- FYSSBMZUBSBFJL-UHFFFAOYSA-N 3-hydroxydecanoic acid Chemical compound CCCCCCCC(O)CC(O)=O FYSSBMZUBSBFJL-UHFFFAOYSA-N 0.000 description 4
- 238000005119 centrifugation Methods 0.000 description 4
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- 229940100890 silver compound Drugs 0.000 description 3
- 150000003379 silver compounds Chemical class 0.000 description 3
- XBUXARJOYUQNTC-UHFFFAOYSA-N ()-3-Hydroxynonanoic acid Chemical compound CCCCCCC(O)CC(O)=O XBUXARJOYUQNTC-UHFFFAOYSA-N 0.000 description 2
- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- KBPLFHHGFOOTCA-UHFFFAOYSA-N 1-Octanol Chemical compound CCCCCCCCO KBPLFHHGFOOTCA-UHFFFAOYSA-N 0.000 description 2
- 229940114072 12-hydroxystearic acid Drugs 0.000 description 2
- JHRQMZPLCYCFPI-UHFFFAOYSA-N 17-hydroxymargaric acid Chemical compound OCCCCCCCCCCCCCCCCC(O)=O JHRQMZPLCYCFPI-UHFFFAOYSA-N 0.000 description 2
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 2
- JDSQBDGCMUXRBM-UHFFFAOYSA-N 2-[2-(2-butoxypropoxy)propoxy]propan-1-ol Chemical compound CCCCOC(C)COC(C)COC(C)CO JDSQBDGCMUXRBM-UHFFFAOYSA-N 0.000 description 2
- LTHNHFOGQMKPOV-UHFFFAOYSA-N 2-ethylhexan-1-amine Chemical compound CCCCC(CC)CN LTHNHFOGQMKPOV-UHFFFAOYSA-N 0.000 description 2
- CPLYLXYEVLGWFJ-UHFFFAOYSA-N 2-hydroxyarachidic acid Chemical compound CCCCCCCCCCCCCCCCCCC(O)C(O)=O CPLYLXYEVLGWFJ-UHFFFAOYSA-N 0.000 description 2
- GHPVDCPCKSNJDR-UHFFFAOYSA-N 2-hydroxydecanoic acid Chemical compound CCCCCCCCC(O)C(O)=O GHPVDCPCKSNJDR-UHFFFAOYSA-N 0.000 description 2
- JGHSBPIZNUXPLA-UHFFFAOYSA-N 2-hydroxyhexadecanoic acid Chemical compound CCCCCCCCCCCCCCC(O)C(O)=O JGHSBPIZNUXPLA-UHFFFAOYSA-N 0.000 description 2
- JYZJYKOZGGEXSX-UHFFFAOYSA-N 2-hydroxymyristic acid Chemical compound CCCCCCCCCCCCC(O)C(O)=O JYZJYKOZGGEXSX-UHFFFAOYSA-N 0.000 description 2
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- CBWALJHXHCJYTE-UHFFFAOYSA-N 3-hydroxypalmitic acid Chemical compound CCCCCCCCCCCCCC(O)CC(O)=O CBWALJHXHCJYTE-UHFFFAOYSA-N 0.000 description 2
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Classifications
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/08—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools with one or more parts not made from powder
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
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- B22F7/00—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression
- B22F7/06—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools
- B22F7/062—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts
- B22F7/064—Manufacture of composite layers, workpieces, or articles, comprising metallic powder, by sintering the powder, with or without compacting wherein at least one part is obtained by sintering or compression of composite workpieces or articles from parts, e.g. to form tipped tools involving the connection or repairing of preformed parts using an intermediate powder layer
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J9/00—Adhesives characterised by their physical nature or the effects produced, e.g. glue sticks
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Abstract
本發明提供下述銀奈米粒子:儘管銀奈米粒子之平均粒徑大到200nm以上,在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高,且比電阻值小。
一種銀奈米粒子,其平均粒徑為200~600nm,且於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。
Description
發明領域
本發明是有關於銀奈米粒子、導電性接著劑、該導電性接著劑之燒結體及構件間具備該燒結體的裝置。
背景技術
以固晶劑等為代表的導電性接著劑是使用在半導體、LED、功率半導體等的接合材料。一般已知的接合方式是藉由利用加壓與加熱的接合、抑或不予加壓而是藉由利用加熱等的燒結來與基材接合。近年來,出於製造程序之簡便性或效率之觀點,持續推展無壓方式的接合材料之開發。
作為無壓方式的接合材料,舉其一為含有環氧樹脂的導電性接著劑。該接合材料是利用低溫處理使環氧樹脂硬化後使用,可抑制空隙之產生抑或提升與基材間之接合強度(專利文獻1)。然而,環氧樹脂本身會形成電阻體,因此,所得導電性或熱傳導性會降低。
另一方面,作為不含環氧樹脂等熱硬化性樹脂的接合材料,近年來一直推展銀奈米粒子之開發。銀奈米粒子具有能利用短時間低溫的熱處理輕易地燒結之特徵。舉例言之,專利文獻2中揭示有一種金屬糊,其係混練
由銀粒子構成的固體成分與溶劑而成,且前述固體成分由銀粒子構成,該銀粒子包含以粒子數基準計為30%以上之粒徑100~200nm的銀粒子,再者,構成固體成分的銀粒子結合了碳數總和為4~8的胺化合物作為保護劑。若藉由該金屬糊,則可於低溫區使銀粒子燒結,並且可形成低電阻的燒結體及熱傳導性優異的燒結體。
先前技術文獻
專利文獻
專利文獻1:國際公開2010/18712號
專利文獻2:日本特開2015-159096號公報
發明概要
如前述,專利文獻2中,若藉由由銀粒子構成之金屬糊,且該金屬糊包含以粒子數基準計為30%以上之粒徑100~200nm的銀粒子,再者,構成固體成分的銀粒子結合了碳數總和為4~8的胺化合物作為保護劑,則可於低溫區使銀粒子燒結,並且可形成低電阻的燒結體及熱傳導性優異的燒結體。
然而,本案發明人進行探討時發現以下問題:在如專利文獻2中所揭示之含有習知銀奈米粒子的金屬糊中,若銀奈米粒子之平均粒徑成為200nm以上,則在例如200℃以下的低溫下使其燒結時燒結體的剪切強度降低,而且比電阻值亦會變大。
於此種狀況下,本發明之主要目的即在於提供下述銀奈米粒子:儘管銀奈米粒子之平均粒徑大到200nm以上,在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高,且比電阻值小。再者,本發明之目的亦在於提供含有該銀奈米粒子的導電性接著劑、該導電性接著劑之燒結體及構件間具備該燒結體的裝置。
本案發明人為了解決上述課題精心探討。結果發現一種銀奈米粒子,其平均粒徑為200~600nm,且於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於預定溫度顯現,利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下,該銀奈米粒子儘管平均粒徑大到200nm以上,在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高,且比電阻值小。本發明是根據此種見解,進一步反覆探討而完成。
即,本發明提供下揭態樣之發明。
第1項.一種銀奈米粒子,其平均粒徑為200~600nm,且於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。
第2項.如第1項之銀奈米粒子,其表面附著有胺化合物。
第3項.一種導電性接著劑,含有如第1項或第2項之銀奈米粒子與溶劑。
第4項.一種燒結體,係如第3項之導電性接著劑之燒結體。
第5項.一種裝置,其係藉由如第4項之燒結體使構件間接合而成。
依據本發明,可提供下述銀奈米粒子:儘管銀奈米粒子之平均粒徑大到200nm以上,在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高,且比電阻值小。再者,依據本發明,亦可提供含有該銀奈米粒子的導電性接著劑、該導電性接著劑之燒結體及構件間具備該燒結體的裝置。
圖1顯示實施例1中合成的銀奈米粒子之SEM相片。
圖2顯示實施例2中合成的銀奈米粒子之SEM相片。
圖3顯示比較例1中使用的銀奈米粒子之SEM相片。
圖4顯示比較例2中使用的銀奈米粒子之SEM相片。
用以實施發明之形態
本發明之銀奈米粒子之特徵在於:平均粒徑為200~600nm,且於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,再者,利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。藉由使本發明之銀奈米粒子具備此種特徵,可發揮以下特性:儘管銀奈米粒子之平均粒徑大到200nm以上,
在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高,且比電阻值小。
以下,詳述本發明之銀奈米粒子、導電性接著劑、該導電性接著劑之燒結體及構件間具備該燒結體的裝置。另,本說明書中,以「~」連結的數值,意指包含將「~」前後的數值設為下限值及上限值的數值範圍。當複數個下限值與複數個上限值個別記載時,可選擇任何下限值與上限值,並以「~」來連結。
1.銀奈米粒子
本發明之銀奈米粒子為含有銀的粒子,平均粒徑為200~600nm。銀奈米粒子之平均粒徑之下限例如為大於200nm,較佳為230nm以上,更佳為250nm以上,上限例如較佳為550nm以下,更佳為500nm以下。
<平均粒徑>
本發明中,銀奈米粒子之平均粒徑是藉由掃描型電子顯微鏡觀察(倍率20,000倍)銀奈米粒子,隨機選擇30個以上存在於視野內的粒子,測定粒徑而算出平均值,設為各自之平均粒徑。
又,本發明之銀奈米粒子中,粒徑100~200nm的粒子數之比率宜小於30%,且以20%以下為佳,以15%以下更佳。即,本發明之銀奈米粒子是要作成儘管平均粒徑大到200nm以上、在低溫下(例如200℃以下)使其燒結時燒結體的剪切強度亦高且比電阻值小的銀奈米粒子,出於此觀點,較為理想的是平均粒徑大到
200~600nm,且粒徑100~200nm的粒子數少。粒徑100~200nm的粒子數之比率,係在前述平均粒徑之測定中隨機選擇30個以上存在於視野內的粒子測定粒徑而求出的值。
又,本發明之銀奈米粒子之特徵在於:於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,且利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。為了將銀奈米粒子之平均粒徑設定在前述範圍,然後更賦予銀奈米粒子此種特性,宜採用後述銀奈米粒子之製造方法。
本發明之銀奈米粒子中所含銀的含量宜為95質量%以上,更佳為98質量%以上。
從進一步地提高在低溫下使其燒結時燒結體的剪切強度並降低比電阻值之觀點來看,前述發熱峰之下限例如較佳為120℃以上,更佳為150℃以上,上限例如較佳為小於175℃,更佳為170℃以下。
又,出於相同觀點,前述重量減少率之下限例如較佳為0.01%重量%以上,更佳為0.05%重量%以上,上限例如較佳為0.3重量%以下,更佳為0.2重量%以下。
<熱重量示差熱分析(TG-DTA)>
首先,準備已風乾的銀奈米粒子。舉例言之,自導電性接著劑取得銀奈米粒子以進行分析時,係對各導電性接著劑1g加入甲醇2g使其充分地分散後,濾出銀奈米粒子加以風乾而得到銀奈米粒子乾燥粉末,作為分析對象。利用
熱重量示差熱分析裝置(例如日立(HITACHI)G300 AST-2),測定銀奈米粒子之乾燥粉末的TG-DTA。測定條件設為環境氣體:空氣、測定溫度:30~500℃、升溫速度:10℃/min。從所得TG-DTA圖表,獲得TG-DTA分析中起因於銀奈米粒子之結合的發熱峰,以及利用熱分析自30℃加熱至500℃時的重量減少率。
又,本發明之銀奈米粒子之微晶尺寸並無特殊限制,下限例如較佳為35nm以上,更佳為40nm以上,上限例如較佳為60nm以下,更佳為50nm以下。本發明之銀奈米粒子之微晶尺寸測定方法如下。
<微晶尺寸之測定>
使用X射線結晶構造解析裝置(例如理學(RIGAKU)Ultima IV),將射線源設為Cu Kα射線,進行X射線結晶構造解析。從所得圖表的(111)峰(2θ=38°)之半值寬,利用謝樂(Scherrer)公式算出微晶尺寸。
為了將銀奈米粒子之平均粒徑設定在前述範圍,然後進一步將銀奈米粒子的前述發熱峰與前述重量減少率(進而為前述微晶尺寸)適當地設定為前述值,宜將銀奈米粒子進行表面處理。即,具備前述物性的本發明之銀奈米粒子宜為表面處理銀奈米粒子。
更具體而言,本發明之銀奈米粒子宜至少於表面附著有胺化合物。胺化合物可附著於銀奈米粒子之表面,並形成保護層。本發明之銀奈米粒子為了將平均粒徑設定在前述特定範圍並具備前述物性,宜使其附著胺化合
物。
胺化合物並無特殊限制,從將銀奈米粒子之平均粒徑設定在前述範圍、然後進一步將銀奈米粒子的前述發熱峰與前述重量減少率適當地設定為前述值之觀點來看,宜為烷基胺。烷基胺並無特殊限制,例如較佳為烷基之碳數為3以上且18以下的烷基胺,更佳為烷基之碳數為4以上且12以下的烷基胺。
烷基胺之較佳具體例可例示:乙胺、n-丙胺、異丙胺、1,2-二甲基丙胺、n-丁胺、異丁胺、sec-丁胺、tert-丁胺、異戊胺、tert-戊胺、3-戊胺、n-戊胺、n-己胺、n-庚胺、n-辛胺、2-辛胺、2-乙基己胺、n-壬胺、n-胺癸烷、n-胺十一烷、n-十二胺、n-十三胺、2-十三胺、n-十四胺、n-十五胺、n-十六胺、n-十七胺、n-十八胺、n-油胺、N-乙基-1,3-二胺丙烷、N,N-二異丙基乙胺、N,N-二甲基胺丙烷、N,N-二丁基胺丙烷、N,N-二甲基-1,3-二胺丙烷、N,N-二乙基-1,3-二胺丙烷、N,N-二異丁基-1,3-二胺丙烷、N-月桂基二胺丙烷等。再者,亦可例示屬於二級胺的二丁胺,抑或屬於環狀烷基胺的環丙胺、環丁胺、環丙胺、環己胺、環庚胺、環辛胺等。該等之中,從有效地提高導電性接著劑之燒結體的機械強度觀點來看,宜為n-丙胺、異丙胺、環丙胺、n-丁胺、異丁胺、sec-丁胺、tert-丁胺、環丁胺、n-戊胺、n-己胺、環己胺、n-辛胺、2-乙基己胺、n-十二胺、n-油胺、N,N-二甲基-1,3-二胺丙烷、N,N-二乙基-1,3-二胺丙烷,且更宜為n-丁胺、n-己胺、環己胺、n-辛胺、n-十
二胺、N,N-二甲基-1,3-二胺丙烷、N,N-二乙基-1,3-二胺丙烷。胺化合物可單獨使用1種,亦可組合使用2種以上。
本發明之銀奈米粒子中,就胺化合物之附著量調整成於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,且利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。具體的胺化合物之附著量只要相對於銀奈米粒子之重量為0.4重量%以下即可,且以0.2重量%以下為佳。附著於銀奈米粒子的胺化合物之含量可利用氣相層析法或熱重量示差熱分析進行測定。
又,銀奈米粒子之表面亦可附著有脂肪酸、羥基脂肪酸等。脂肪酸並無特殊限制,例如較佳為烷基之碳數為3以上且18以下的脂肪酸,更佳為烷基之碳數為4以上且18以下的脂肪酸。脂肪酸之較佳具體例可列舉如:乙酸、丙酸、丁酸、戊酸、己酸、辛酸、2-乙基己酸、癸酸、月桂酸、肉豆蔻酸、軟脂酸、硬脂酸、油酸、亞麻油酸、α-次亞麻油酸等。又,脂肪酸之具體例亦可舉例像是環己烷羧酸之環狀烷基羧酸等。又,羥基脂肪酸可使用碳數3~24且具有1個以上(例如1個)羥基的化合物。又,羥基脂肪酸例如可列舉:2-羥癸酸、2-羥十二酸、2-羥十四酸、2-羥十六酸、2-羥十八酸、2-羥二十酸、2-羥二十二酸、2-羥二十三酸、2-羥二十四酸、3-羥己酸、3-羥辛酸、3-羥壬酸、3-羥癸酸、3-羥十一酸、3-羥十二酸、3-羥十三酸、3-羥十四酸、3-羥十六酸、3-羥十七酸、3-羥十八酸、ω-羥
基-2-癸烯酸、ω-羥十五酸、ω-羥十七酸、ω-羥二十酸、ω-羥二十二酸、6-羥十八酸、蓖麻油酸、12-羥硬脂酸、[R-(E)]-12-羥基-9-十八烯酸等。其中又以碳數4~18且ω位以外(特別是12位)具有1個羥基的羥基脂肪酸為佳,且以蓖麻油酸、12-羥硬脂酸更佳。脂肪酸及羥基脂肪酸可分別單獨使用1種,亦可組合使用2種以上。
本發明之銀奈米粒子中,針對脂肪酸或羥基脂肪酸之附著量亦與胺化合物相同,調整成於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,且利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下。具體的脂肪酸或羥基脂肪酸之附著量只要相對於銀奈米粒子之重量為0.3重量%以下即可,且以0.1重量%以下為佳。附著於銀奈米粒子的脂肪酸或羥基脂肪酸之含量可利用氣相層析法或熱重量示差熱分析進行測定。
另,以本發明之銀奈米粒子滿足前述平均粒徑與物性為限,亦可併用胺化合物、脂肪酸、羥基脂肪酸,又,與該等不同的其他化合物亦可附著於銀奈米粒子之表面。從將本發明之銀奈米粒子之平均粒徑設定在前述範圍、然後更賦予銀奈米粒子前述物性之觀點來看,本發明之銀奈米粒子之表面附著有胺化合物是特別理想的。
2.銀奈米粒子之製造方法
以下顯示本發明之銀奈米粒子之製造方法的一例。
首先,準備用以製造銀奈米粒子的組成物(銀
奈米粒子調製用組成物)。具體而言,準備成為銀奈米粒子原料的銀化合物,以及視需要而定的附著於銀奈米粒子表面的胺化合物等或溶劑。為了將本發明之銀奈米粒子之平均粒徑設定在前述範圍,然後更賦予銀奈米粒子前述物性,理想的銀化合物可列舉硝酸銀、草酸銀等,特別是以草酸銀為佳。另,溶劑可例示與針對後述導電性接著劑中摻合之溶劑所例示者相同的溶劑。其次,混合該等各成分,製得銀奈米粒子調製用組成物。該組成物中各成分之比率可適當地調整。舉例言之,組成物中草酸銀之含量宜相對於組成物之總量設為20~70質量%。又,若為使銀奈米粒子表面附著胺化合物之情形,則胺化合物之含量宜相對於組成物之總量設為5質量%~55質量%。又,若為使銀奈米粒子表面附著脂肪酸之情形,則脂肪酸之含量宜相對於組成物之總量設為0.1質量%~20質量%。若為使銀奈米粒子表面附著羥基脂肪酸之情形,則羥基脂肪酸之含量宜相對於組成物之總量設為0.1質量%~15質量%。
另,亦可使用調整成胺化合物等之含量在前述範圍外的銀奈米粒子調製用組成物,暫時合成銀奈米粒子,並藉由後述方法,對胺化合物等之種類或附著量進行調整(取代胺化合物)以成為前述物性。
又,各成分之混合機構亦無特殊限制,例如可藉由機械攪拌器、磁攪拌器、旋渦混合器、行星式磨機、球磨機、三輥機、管線混合器、行星式混合器、溶解器等通用裝置進行混合。為了避免因混合時的溶解熱、摩擦熱
等影響使組成物之溫度上升,以致銀奈米粒子開始熱解反應,宜在將組成物之溫度抑制在例如60℃以下、特別是40℃以下的狀態下進行混合。
其次,將銀奈米粒子調製用組成物供於反應容器內反應,通常為利用加熱的反應,藉此引起銀化合物的熱解反應,並生成銀奈米粒子。反應時,可將組成物導入至已預先加熱的反應容器內,亦可將組成物導入至反應容器內後再進行加熱。
反應溫度只要是可進行熱解反應並生成銀奈米粒子的溫度即可,可舉例如50~250℃。又,反應時間配合期望平均粒徑的大小抑或因應其之組成物的組成適當地選擇即可。反應時間可舉例如1分鐘~100小時。
利用熱解反應生成的銀奈米粒子會以含有未反應原料之混合物之形式獲得,因此,宜將銀奈米粒子進行精製。精製方法可列舉如:固液分離方法、利用銀奈米粒子與有機溶劑等未反應原料之比重差的沈澱方法等。固液分離方法可列舉如:過濾器過濾、離心分離、旋風式或傾析器等方法。為使精製時處理容易,亦可利用丙酮、甲醇等低沸點溶劑稀釋含有銀奈米粒子的混合物來調整其黏度。
藉由調整銀奈米粒子製造用組成物的組成或反應條件,可調整所得銀奈米粒子之平均粒徑。
取代、調整銀奈米粒子表面的胺化合物之方法
準備已利用前述方法暫時合成的銀奈米粒子(表面附著有胺化合物),使其分散於溶劑中。溶劑可例示與針對後述導電性接著劑中摻合之溶劑所例示者相同的溶劑。其次,以相對於銀奈米粒子之質量為0.1~5倍量的範圍添加其他胺化合物,並在室溫~80℃下攪拌1分~24小時,藉由交付於該步驟,可取代附著於銀奈米粒子表面的胺化合物之種類或是調整附著量。經取代胺化合物的銀奈米粒子可藉由前述固液分離法等進行回收。
3.導電性接著劑
本發明之導電性接著劑之特徵在於:含有本發明之銀奈米粒子與溶劑。藉由含有溶劑,流動性提高,可輕易地將本發明之導電性接著劑配置在期望之場所。本發明之銀奈米粒子之詳情如前述。
溶劑只要是可將銀奈米粒子分散,則無特殊限制,宜含有極性有機溶劑。極性有機溶劑可列舉如:丙酮、乙醯丙酮、甲基乙基酮等酮類;二乙基醚、二丙基醚、二丁基醚、四氫呋喃、1,4-二噁烷等醚類;1,2-丙二醇、1,2-丁二醇、1,3-丁二醇、1,4-丁二醇、2,3-丁二醇、1,2-己二醇、1,6-己二醇、1,2-戊二醇、1,5-戊二醇、2-甲基-2,4-戊二醇、3-甲基-1,5-戊二醇、1,2-辛二醇、1,8-辛二醇、2-乙基-1,3-己二醇等二醇類;丙三醇;碳數1~5之直鏈或支鏈的醇、環己醇、3-甲氧基-3-甲基-1-丁醇、3-甲氧基-1-丁醇等醇類;乙酸乙酯、乙酸丁酯、丁酸乙酯、甲酸乙酯等脂肪酸酯類;聚乙二醇、三乙二醇單甲基醚、四乙二醇單
甲基醚、乙二醇單乙基醚、二乙二醇單乙基醚、二乙二醇二甲基醚、三乙二醇二甲基醚、四乙二醇二甲基醚、3-甲氧丁基乙酸酯、乙二醇單丁基醚、乙二醇單丁基醚乙酸酯、乙二醇單己基醚、乙二醇單辛基醚、乙二醇單-2-乙基己基醚、乙二醇單苄基醚、二乙二醇單甲基醚、二乙二醇單甲基醚乙酸酯、二乙二醇單乙基醚、二乙二醇單乙基醚乙酸酯、二乙二醇單丁基醚、二乙二醇單丁基醚乙酸酯、二乙二醇單己基醚、二乙二醇單-2-乙基己基醚、聚丙二醇、丙二醇單丙基醚、丙二醇單丁基醚、二丙二醇單甲基醚、二丙二醇單乙基醚、二丙二醇單丙基醚、二丙二醇單丁基醚、三丙二醇單甲基醚、三丙二醇單乙基醚、三丙二醇單丙基醚、三丙二醇單丁基醚等二醇或二醇醚類;N,N-二甲基甲醯胺;二甲亞碸;萜品醇等萜類;乙腈;γ-丁內酯;2-吡咯啶酮;N-甲基吡咯啶酮;N-(2-胺乙基)哌嗪等。該等之中,從更進一步有效地提高導電性接著劑之燒結體的機械強度觀點來看,宜為碳數3~5之直鏈或支鏈的醇、3-甲氧基-3-甲基-1-丁醇、3-甲氧基-1-丁醇、二乙二醇單丁基醚、二乙二醇單丁基醚乙酸酯、萜品醇。
溶劑除了極性有機溶劑外,更可含有非極性或疏水性溶劑。非極性有機溶劑可列舉如:己烷、庚烷、辛烷、壬烷、癸烷、2-乙基己烷、環己烷等直鏈、分枝或環狀飽和烴;碳數6以上之直鏈或支鏈的醇等醇類;苯、甲苯、苄腈等芳香族化合物;二氯甲烷、氯仿、二氯乙烷等鹵化烴類;甲基-n-戊基酮;甲基乙基酮肟;甘油三乙酸酯
等。該等之中又以飽和烴及碳數6以上之直鏈或支鏈的醇類為佳,且以己烷、辛烷、癸烷、辛醇、癸醇、十二醇更佳。溶劑可單獨1種或混合2種以上使用。
當含有極性有機溶劑與非極性有機溶劑兩者時,極性有機溶劑之比率相對於溶劑之總量宜為5容量%以上,較佳為10容量%以上,更佳為15容量%以上。又,可設為60容量%以下,亦可設為55容量%以下,也可以設為50容量%以下。溶劑亦可設為僅由極性有機溶劑構成。本發明之導電性接著劑在依此含有許多極性有機溶劑時,銀奈米粒子之分散性亦良好。
本發明之導電性接著劑中,溶劑之比率並無特殊限制,宜為20質量%以下,且以5質量%~15質量%更佳。
本發明之導電性接著劑中所含銀奈米粒子之含量宜為80質量%以上,更佳為85質量%以上。
本發明之導電性接著劑可利用具備以下步驟的方法來製造,所述步驟係混合本發明之銀奈米粒子與溶劑。
又,本發明之導電性接著劑之製造方法中,亦可將前述本發明之銀奈米粒子之製造方法中在溶劑中生成的本發明之銀奈米粒子,與溶劑一同作成本發明之導電性接著劑。
4.導電性接著劑之燒結體
本發明之導電性接著劑之燒結體,可藉由將前述「2.
導電性接著劑」中詳述之本發明導電性接著劑燒結而製得。本發明之導電性接著劑之燒結體中,附著於銀奈米粒子表面的成分(胺化合物等)、溶劑會因燒結時的高熱而幾乎脫離,燒結體實質上由銀構成。
燒結溫度並無特殊限制,從所製得之燒結體發揮高導電性與高接著力並有效地提高機械強度的觀點來看,例如較佳為150℃~200℃左右,更佳為150℃~185℃左右。出於相同觀點,燒結時間例如較佳為0.4小時~2.0小時左右,更佳為0.5小時~1.2小時左右。習知粒徑大的銀奈米粒子(例如平均粒徑為200nm以上)在200℃以下的低溫下使其燒結時,燒結會變得不完全,難以製得剪切強度高且比電阻值小的燒結體,但藉由使用含有本發明之銀奈米粒子的導電性接著劑,就可製得下述燒結體:儘管銀奈米粒子之平均粒徑大到200nm以上、在200℃以下的低溫下使其燒結時燒結體之剪切強度亦高且比電阻值小的燒結體。燒結可於大氣、非活性氣體(氮氣、氬氣)等環境氣體下進行。燒結機構並無特殊限制,可列舉如:烘箱、熱風式乾燥爐、紅外線乾燥爐、雷射照射、閃光燈照射、微波等。
又,本發明之燒結體之微晶尺寸並無特殊限制,下限例如較佳為75nm以上,更佳為80nm以上,上限例如較佳為95nm以下,更佳為90nm以下。本發明之燒結體之微晶尺寸測定方法與前述銀奈米粒子之微晶尺寸測定方法相同。
5.裝置
本發明之裝置具備藉由本發明之燒結體使構件間接著的部分。即,本發明之裝置係將前述「2.導電性接著劑」中詳述之本發明導電性接著劑配置於裝置之構件間(例如電路所含之構件間),且使導電性接著劑燒結而將構件間予以接著。
如前述,本發明之燒結體的剪切強度高,且比電阻值小,因此,在具備其的裝置或電路中,構件間的剪切強度亦高,且比電阻值小。
實施例
以下實施例中更具體說明本發明,惟本發明並不限於該等。
實施例及比較例中使用的各成分之詳情如下。
.草酸銀((COOAg)2)是藉由日本專利第5574761號公報中記載的方法來合成。
.N,N-二乙基-1,3-二胺丙烷(和光純藥工業股份有限公司製造)
.2-(2-胺基乙氧基)乙醇(和光純藥工業股份有限公司製造)
.n-己胺(碳數6,和光純藥工業股份有限公司製造)
.丁醇(和光純藥工業股份有限公司製造)
.甲醇(和光純藥工業股份有限公司製造)
.比較例1之銀奈米粒子使用都華(DOWA)電子股份
有限公司製造之製品名AG 2-1C。
.比較例2之銀奈米粒子使用德力本店股份有限公司製造之製品名AGS-050。
<實施例1>
在已放入磁攪拌棒的50mL玻璃製離心管中,投入N,N-二乙基-1,3-二胺丙烷(1.72g)、2-(2-胺基乙氧基)乙醇(1.39g)及丁醇(6.0g),攪拌1分鐘後,投入草酸銀(4.0g),攪拌約10分鐘,藉此,製得銀奈米粒子調製用組成物。然後,將該等玻璃製離心管直立設置於具備鋁塊的加熱攪拌器(小池精密機器製作所製造HHE-19G-U)上,於40℃下攪拌30分鐘,再於90℃下攪拌30分鐘。放冷後,取出磁攪拌棒,並於各組成物中添加甲醇15g,利用旋渦混合器攪拌後,藉由離心分離機(日立工機製造CF7D2),以3000rpm(約1600×G)實施1分鐘離心操作,藉由使離心管傾斜,除去上澄液。反覆2次甲醇15g之添加、攪拌、離心分離及上澄液除去步驟,回收所製造的銀奈米粒子A。
(胺化合物之取代)
使用上述中製得的銀奈米粒子A之分散液(甲醇溶液),與銀奈米粒子之質量等量添加n-己胺,於室溫下攪拌4小時。攪拌後,取出磁攪拌棒,並於各組成物中添加甲醇15g,利用旋渦混合器攪拌後,藉由離心分離機(日立工機製造CF7D2),以3000rpm(約1600×G)實施1分鐘離心操作,藉由使離心管傾斜,除去上澄液。反覆2次甲醇15g之添加、攪拌、離心分離及上澄液除去步驟,回收已調整(取
代)保護層中胺比率的實施例1之銀奈米粒子1。
<實施例2>
在已放入磁攪拌棒的50mL玻璃製離心管中,投入2-(2-胺基乙氧基)乙醇(2.91g)及丁醇(6.0g),攪拌1分鐘後,投入草酸銀(4.0g),攪拌約10分鐘,藉此,製得銀奈米粒子調製用組成物。然後,將該等玻璃製離心管直立設置於具備鋁塊的加熱攪拌器(小池精密機器製作所製造HHE-19G-U)上,於40℃下攪拌30分鐘,再於90℃下攪拌30分鐘。放冷後,取出磁攪拌棒,並於各組成物中添加甲醇15g,利用旋渦混合器攪拌後,藉由離心分離機(日立工機製造CF7D2),以3000rpm(約1600×G)實施1分鐘離心操作,藉由使離心管傾斜,除去上澄液。反覆2次甲醇15g之添加、攪拌、離心分離及上澄液除去步驟,回收所製造的銀奈米粒子B。
(胺化合物之取代)
取代銀奈米粒子A,銀奈米粒子A亦設為與前述銀奈米粒子A相同,回收實施例2之銀奈米粒子2。
<平均粒徑之測定>
藉由掃描型電子顯微鏡(基恩斯(KEYENCE)製造VE-7800,日立先端科技製造S-4500),觀察(倍率20,000倍)實施例1、2及比較例1、2的各銀奈米粒子,隨機選擇30個存在於視野內的粒子,測定粒徑而算出平均值,設為各自之平均粒徑。表1中顯示結果。
<導電性接著劑之製造>
使用實施例1、2及比較例1、2的各銀奈米粒子,添加十二碳醇酯(TEXANOL),使銀含量構成85質量%,製得各銀奈米粒子分散液。分別使用倉敷紡績(KURABO)公司製造之MAZERUSTAR,以2次攪拌優先模式混合該等液體,調製出各導電性接著劑。
<熱重量示差熱分析(TG-DTA)>
對各導電性接著劑1g加入甲醇2g使其充分地分散後,濾出銀奈米粒子加以風乾而得到銀奈米粒子乾燥粉末。利用日立(HITACHI)G300 AST-2,測定該乾燥粉末的TG-DTA。測定條件設為環境氣體:空氣、測定溫度:30~500℃、升溫速度:10℃/min。從所得TG-DTA圖表,獲得TG-DTA分析中起因於銀奈米粒子之結合的發熱峰,以及利用熱分析自30℃加熱至500℃時的重量減少率。表1中顯示結果。
<微晶尺寸之測定>
使用理學(RIGAKU)Ultima IV(射線源:Cu Kα射線),對各銀奈米粒子與各導電性接著劑之燒結體(以200℃、60分鐘之燒結條件製得的塗膜)的平均微晶尺寸進行X射線結晶構造解析。從所得圖表的(111)峰(2θ=38°)之半值寬,利用謝樂(Scherrer)公式算出微晶尺寸。表1中顯示結果。
<塗膜(燒結體)的剪切強度之測定>
準備銅板上已施行無電鍍銀0.5μm的基材,使用金屬遮罩將各導電性接著劑以塗膜厚度成為50μm之方式在該
基材上均勻地形成塗膜。於塗膜上,使背面(與導電性接著劑相接的面)已施行鍍金或金濺鍍處理的矽晶圓(尺寸2mm×2mm)載置於上方。其次,使用乾燥器(循環式),以預定燒結條件(175℃、30分鐘或200℃、60分鐘)進行加熱,製得各導電性接著劑已燒結的塗膜(燒結體)。所得各塗膜(燒結體)的剪切強度是使用黏結強度試驗機(西進商事製造SS30-WD)實施晶粒剪切試驗進行測定。表1中顯示測定結果。
<塗膜的比電阻值之測定>
使用金屬遮罩將各導電性接著劑分別以在聚醯亞胺膜上構成2mm×60mm×50μm之方式形成塗膜。其次,以預定燒結條件(175℃、30分鐘或200℃、60分鐘)進行加熱,製得各導電性接著劑已燒結的塗膜(燒結體)。利用電阻計(日置(HIOKI)RM3548)測定燒結體的電阻值,求出比電阻值。表1中顯示結果。
如表1所示,由使用了TG-DTA發熱峰小於175℃且TG-DTA重量減少量為0.4重量%以下的各銀奈米粒子(實施例1與實施例2)之導電性接著劑製得的塗膜,相較於使用了TG-DTA發熱峰高於175℃且TG-DTA重量減少量大於0.4重量%的粒子之導電性接著劑,顯示出高剪切強度與低比電阻值。
Claims (5)
- 一種銀奈米粒子,其平均粒徑為200~600nm,且於熱重量示差熱分析中起因於銀奈米粒子之結合的發熱峰以小於175℃顯現,利用熱重量示差熱分析自30℃加熱至500℃時的重量減少率為0.4重量%以下;該熱重量示差熱分析之測定條件係設為環境氣體:空氣、升溫速度:10℃/min。
- 如請求項1之銀奈米粒子,其表面附著有胺化合物。
- 一種導電性接著劑,含有如請求項1或2之銀奈米粒子與溶劑。
- 一種燒結體,係如請求項3之導電性接著劑之燒結體。
- 一種構件間具備燒結體的裝置,其係藉由如請求項4之燒結體使構件間接合而成。
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