JP2010055788A - Silver paste - Google Patents
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- JP2010055788A JP2010055788A JP2008216559A JP2008216559A JP2010055788A JP 2010055788 A JP2010055788 A JP 2010055788A JP 2008216559 A JP2008216559 A JP 2008216559A JP 2008216559 A JP2008216559 A JP 2008216559A JP 2010055788 A JP2010055788 A JP 2010055788A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 44
- 239000004332 silver Substances 0.000 title claims abstract description 44
- 239000003822 epoxy resin Substances 0.000 claims abstract description 31
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 20
- 229920003986 novolac Polymers 0.000 claims abstract description 18
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims abstract description 14
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 12
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 12
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000005642 Oleic acid Substances 0.000 claims abstract description 12
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 12
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 12
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 229920001187 thermosetting polymer Polymers 0.000 abstract description 10
- 238000005476 soldering Methods 0.000 abstract description 3
- 239000010408 film Substances 0.000 description 9
- 238000007650 screen-printing Methods 0.000 description 7
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 5
- 229910000679 solder Inorganic materials 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920005989 resin Polymers 0.000 description 4
- 239000011347 resin Substances 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 description 2
- WTEOIRVLGSZEPR-UHFFFAOYSA-N boron trifluoride Chemical compound FB(F)F WTEOIRVLGSZEPR-UHFFFAOYSA-N 0.000 description 2
- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
- SLGWESQGEUXWJQ-UHFFFAOYSA-N formaldehyde;phenol Chemical compound O=C.OC1=CC=CC=C1 SLGWESQGEUXWJQ-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 description 1
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 description 1
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 description 1
- TYOXIFXYEIILLY-UHFFFAOYSA-N 5-methyl-2-phenyl-1h-imidazole Chemical compound N1C(C)=CN=C1C1=CC=CC=C1 TYOXIFXYEIILLY-UHFFFAOYSA-N 0.000 description 1
- 229910015900 BF3 Inorganic materials 0.000 description 1
- 229930185605 Bisphenol Natural products 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 239000000306 component Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000001723 curing Methods 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000009429 electrical wiring Methods 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 230000003628 erosive effect Effects 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- -1 glycidyl ester Chemical class 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 150000007517 lewis acids Chemical class 0.000 description 1
- XLSZMDLNRCVEIJ-UHFFFAOYSA-N methylimidazole Natural products CC1=CNC=N1 XLSZMDLNRCVEIJ-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Abstract
Description
本発明は、電気配線又は電極の形成に用いられる加熱硬化型銀ペーストであって、はんだ付け性に優れ且つスクリーン印刷性が良好な銀ペーストに関するものである。 The present invention relates to a heat-curable silver paste used for forming an electrical wiring or an electrode, and relates to a silver paste having excellent solderability and good screen printability.
従来、高温で処理すると特性が劣化してしまうような電気配線基板や電子部品の配線又は電極を形成する方法としては、銀、アルミニウム等のスパッタリングや蒸着による薄膜方式と、加熱硬化型ペーストを用いる厚膜方式がよく知られている。 Conventionally, as a method for forming wiring or electrodes of electric wiring boards and electronic parts whose characteristics deteriorate when treated at high temperatures, a thin film method by sputtering or vapor deposition of silver, aluminum, etc., and a thermosetting paste are used. Thick film systems are well known.
そのうちの厚膜方式は、加熱硬化型銀ペーストを基板や部品等に塗布又は印刷した後、２５０℃以下の低温で加熱して乾燥、硬化させることにより、配線又は電極を形成するものである。この厚膜方式は、設備が安価で、生産性も高いことから、フィルムアンテナ等の配線やコンデンサ、抵抗器、太陽電池等の電極の製造に広範に利用されている。 In the thick film method, a wiring or an electrode is formed by applying or printing a thermosetting silver paste on a substrate or a component, and then heating and drying and curing at a low temperature of 250 ° C. or lower. Since this thick film system is inexpensive and has high productivity, it is widely used for manufacturing wiring for film antennas, electrodes for capacitors, resistors, solar cells, and the like.
ところで、上記厚膜方式に用いる加熱硬化型銀ペーストは、銀粉末と、エポキシ樹脂などの加熱硬化性樹脂と、溶剤とで実質的に構成される。導電粉末として銀粉末が用いられるのは、銀は電気抵抗が小さく、酸化され難いうえ、金に比べて安価であるなどの理由による。 By the way, the thermosetting silver paste used in the thick film system is substantially composed of silver powder, a thermosetting resin such as an epoxy resin, and a solvent. The reason why silver powder is used as the conductive powder is that silver has low electrical resistance, is not easily oxidized, and is cheaper than gold.
上記厚膜方式に用いられる加熱硬化型銀ペーストについては、従来から数多くの研究と提案されている。例えば特開平０８−０９２５０６号公報には、銀粉末と、エポキシ樹脂及びそのイミダゾール系硬化剤とを含み、はんだ付け性が良好で且つ十分な引張強度を有する加熱硬化型銀ペーストが提案されている。 Many studies have been proposed for the thermosetting silver paste used in the thick film system. For example, Japanese Patent Application Laid-Open No. 08-092506 proposes a thermosetting silver paste containing silver powder, an epoxy resin and its imidazole curing agent, having good solderability and sufficient tensile strength. .
しかしながら、上記の加熱硬化型銀ペーストは、半硬化状態にしてはんだ付け性を確保するものである。即ち、はんだ付け性と接着強度を十分なものにするためには、硬化条件を限定しなければならないという問題があった。
本発明は、上記した従来の事情に鑑み、硬化条件を限定する必要がなく、十分に硬化させた状態でもはんだ付けが可能であると共に、配線などの微細化に伴って要求されているスクリーン印刷性についても良好な熱硬化型銀ペーストを提供することを目的とする。 In view of the above-described conventional circumstances, the present invention is not required to limit the curing conditions, and can be soldered even in a sufficiently cured state, and screen printing is required along with miniaturization of wiring and the like. The object is to provide a thermosetting silver paste that is also good in properties.
上記目的を達成するため、本発明が提供する銀ペ−ストは、銀粉末と、エポキシ樹脂及びその硬化剤と、溶剤とを含む加熱硬化型銀ペーストであって、エポキシ樹脂の硬化剤がフェノールノボラック化合物であり、更にオレイン酸を銀粉末に対し０.０５〜０.５重量％含むことを特徴とする。 In order to achieve the above object, a silver paste provided by the present invention is a heat curable silver paste containing silver powder, an epoxy resin and its curing agent, and a solvent, and the curing agent of the epoxy resin is phenol. It is a novolak compound and further contains 0.05 to 0.5% by weight of oleic acid with respect to the silver powder.
本発明によれば、銀ペーストにおけるエポキシ樹脂の硬化剤としてフェノールノボラック化合物硬化剤を用い、更にオレイン酸を添加配合することにより、スクリーン印刷性が良好であると同時に、はんだ付け性に優れ、硬化させた状態でもはんだ付けが可能な熱硬化型銀ペーストを提供することができる。 According to the present invention, a phenol novolac compound curing agent is used as a curing agent for the epoxy resin in the silver paste, and oleic acid is added and blended. It is possible to provide a thermosetting silver paste that can be soldered even in such a state.
本発明が提供する銀ペーストは、厚膜方式により配線や電極を形成するための熱硬化型銀ペーストであって、導電粉末としての銀粉末と、エポキシ樹脂及びその硬化剤としてのフェノールノボラック化合物と、溶剤とで実質的に構成されると共に、更にオレイン酸を少量添加配合することによってペーストの粘度が大きく低下し、特に良好なスクリーン印刷性が得られるものである。 The silver paste provided by the present invention is a thermosetting silver paste for forming wirings and electrodes by a thick film method, and includes silver powder as a conductive powder, an epoxy resin and a phenol novolak compound as a curing agent thereof. In addition to being substantially composed of a solvent, and further adding and mixing a small amount of oleic acid, the viscosity of the paste is greatly reduced, and particularly good screen printability is obtained.
本発明の銀ペーストにおけるオレイン酸の含有量は、銀粉末に対して０.０５〜０.５重量％の範囲とする。オレイン酸の量が０.０５重量％未満では、銀ペーストの粘度が高くなり過ぎ、スクリーン印刷時に版抜けが悪くなってしまう。また、オレイン酸の量が０.５重量％を越えると、銀ペーストの粘度が低くなり過ぎるため、スクリーン印刷時にパターンが滲んでしまう。 The content of oleic acid in the silver paste of the present invention is in the range of 0.05 to 0.5% by weight with respect to the silver powder. If the amount of oleic acid is less than 0.05% by weight, the viscosity of the silver paste becomes too high, and the plate slippage becomes worse during screen printing. On the other hand, if the amount of oleic acid exceeds 0.5% by weight, the viscosity of the silver paste becomes too low, and the pattern is blurred during screen printing.
また、本発明の銀ペーストでは、エポキシ樹脂と、その硬化剤としてフェノールノボラック化合物を用いることによって、良好なはんだ付け性と引張強度が得られるだけでなく、はんだ付けの硬化条件が限定されず、はんだ付けが銀ペーストを十分に硬化させた状態でも可能になる。 Moreover, in the silver paste of the present invention, by using a phenol novolac compound as an epoxy resin and its curing agent, not only good solderability and tensile strength can be obtained, but also the curing conditions for soldering are not limited, Soldering is possible even when the silver paste is sufficiently cured.
使用するエポキシ樹脂としては、特に制限はなく、主に電子材料の成形や接着あるいは封止などに通常用いられているものであってよい。例えば、ビスフェノールＡ型エポキシ樹脂やビスフェノールＦ型エポキシ樹脂のようなビスフェノール型エポキシ樹脂などの２感応型エポキシ樹脂、フェノールノボラック型エポキシ樹脂などの多官能型エポキシ樹脂、ビフェニル型エポキシ樹脂、グリシジルエステル型エポキシ樹脂、脂環式エポキシ樹脂などを用いることができる。また、これらのエポキシ樹脂は、単独でも複数を混合して用いても差し支えない。 There is no restriction | limiting in particular as an epoxy resin to be used, You may use what is normally used mainly for shaping | molding of an electronic material, adhesion | attachment, sealing. For example, two-sensitive epoxy resins such as bisphenol type epoxy resins such as bisphenol A type epoxy resin and bisphenol F type epoxy resin, polyfunctional type epoxy resins such as phenol novolac type epoxy resin, biphenyl type epoxy resin, glycidyl ester type epoxy Resins, alicyclic epoxy resins, and the like can be used. These epoxy resins may be used alone or in combination.
エポキシ樹脂の硬化剤としては、フェノールノボラック化合物を用いる。好ましいフェノールノボラック化合物としては、フェノールホルムアルデヒド型ノボラック樹脂、フェノールアラルキル型ノボラック樹脂などを挙げることができる。硬化剤としてフェノールノボラック化合物を用いることにより、はんだ付け性及び引張強度の向上と共に、他の硬化剤に比べて銀ペーストで形成した配線や電極の抵抗値を低くすることができる。尚、フェノールノボラック化合物硬化剤の量は、使用したエポキシ樹脂を硬化条件下で十分硬化できる量であれば良い。 A phenol novolac compound is used as a curing agent for the epoxy resin. Preferable phenol novolak compounds include phenol formaldehyde type novolak resins and phenol aralkyl type novolak resins. By using a phenol novolak compound as a curing agent, it is possible to improve the solderability and the tensile strength, and to lower the resistance value of wirings and electrodes formed of silver paste as compared with other curing agents. The amount of the phenol novolac compound curing agent may be an amount that can sufficiently cure the used epoxy resin under curing conditions.
エポキシ樹脂とフェノールノボラック化合物硬化剤の含有量は、銀粉末１００重量部に対し、合計で０.６〜２．５重量部配合することが好ましい。エポキシ樹脂とフェノールノボラック化合物硬化剤の合計が０.６重量部未満では、接着強度が低下し且つはんだ喰われが起こりやすい。また、エポキシ樹脂とフェノールノボラック化合物硬化剤の合計が２.５重量部を越えると、はんだ付け性が極端に低下するため好ましくない。 The total content of the epoxy resin and the phenol novolac compound curing agent is preferably 0.6 to 2.5 parts by weight with respect to 100 parts by weight of the silver powder. When the total of the epoxy resin and the phenol novolac compound curing agent is less than 0.6 parts by weight, the adhesive strength is lowered and solder erosion is likely to occur. On the other hand, if the total of the epoxy resin and the phenol novolak compound curing agent exceeds 2.5 parts by weight, the solderability is extremely lowered, which is not preferable.
銀ペーストに用いる銀粉末については、特に制限はなく、球状又はフレーク状のいずれか片方若しくは両方を用いることができる。銀粉末の平均粒径は、特に制限されないが、２０μｍ以下が望ましい。平均粒径が２０μｍを越えると、スクリーン印刷時に目詰まりが発生したり、接着強度が低下したりしてしまうからである。 There is no restriction | limiting in particular about the silver powder used for a silver paste, Either one or both of spherical shape or flake shape can be used. The average particle size of the silver powder is not particularly limited, but is preferably 20 μm or less. This is because if the average particle size exceeds 20 μm, clogging may occur during screen printing, or the adhesive strength may decrease.
溶剤としては、特に限定されるものではなく、ペーストに一般的に用いられている溶剤を用いることができる。具体的には、メチルカルビトール、ブチルカルビトール、ブチルカルビトールアセテート、ジエチレングリコール、プロピレングリコール等を好適に用いることができる。溶剤の含有量は、銀粉末の均一な分散が可能であり、且つ銀ペーストのスクリーン印刷可能な粘度が得られる量であれば良い。 The solvent is not particularly limited, and a solvent generally used for pastes can be used. Specifically, methyl carbitol, butyl carbitol, butyl carbitol acetate, diethylene glycol, propylene glycol and the like can be suitably used. The content of the solvent may be an amount that can uniformly disperse the silver powder and can obtain a screen-printable viscosity of the silver paste.
更に、本発明の銀ペーストでは、硬化を促進させることを目的として、メチルイミダゾールなどのイミダゾール類、アミン類、三フッ化ホウ素を含むルイス酸錯体などの硬化促進剤を配合することができる。硬化促進剤の含有量は、エポキシ樹脂１００重量部に対して１０重量部以下とすることが好ましい。 Furthermore, in the silver paste of this invention, hardening accelerators, such as Lewis acid complexes containing imidazoles, such as methyl imidazole, amines, and boron trifluoride, can be mix | blended for the purpose of accelerating hardening. The content of the curing accelerator is preferably 10 parts by weight or less with respect to 100 parts by weight of the epoxy resin.
尚、本発明の銀ペーストの製造は、上記した銀粉末、エポキシ樹脂、硬化剤のフェノールノボラック化合物、溶剤、及びオレイン酸の各成分、必要に応じて硬化促進剤を、ロールミルなどの市販の混練装置を用いて通常のごとく混練すればよい。 The production of the silver paste of the present invention involves the above-described silver powder, epoxy resin, phenol novolac compound of a curing agent, solvent, and components of oleic acid, and optionally a curing accelerator, a commercially available kneading machine such as a roll mill. What is necessary is just to knead as usual using an apparatus.
銀粉末として、平均粒径が１.９μｍの球状粉末と平均粒径が７.６μｍのフレーク状粉末を用いた。エポキシ樹脂としてビスフェノールＡ型エポキシ樹脂（エポキシ当量１９０）、硬化剤としてフェノールホルムアルデヒド型ノボラック樹脂（水酸基当量１０４）を用いた。硬化促進剤として２−フェニル−４−メチルイミダゾ−ルを少量加えた。溶剤にはジプロピレングリコールを用いた。 As the silver powder, a spherical powder having an average particle diameter of 1.9 μm and a flaky powder having an average particle diameter of 7.6 μm were used. A bisphenol A type epoxy resin (epoxy equivalent 190) was used as an epoxy resin, and a phenol formaldehyde type novolak resin (hydroxyl equivalent 104) was used as a curing agent. A small amount of 2-phenyl-4-methylimidazole was added as a curing accelerator. Dipropylene glycol was used as the solvent.
上記の各成分を下記表１に示す配合割合で混合し、更にオレイン酸を試料ごとに配合割合を変えて添加した。尚、全ての試料において銀粉は、６７.５０重量部の球状粉末と２２.５０重量部のフレーク状粉末とを混合して、銀粉末１００重量部とした。これらを３本ロールミルで混練して、試料１〜８の銀ペーストをそれぞれ作製した。 Each of the above components was mixed at the blending ratio shown in Table 1 below, and oleic acid was added at different blending ratios for each sample. In all samples, the silver powder was mixed with 67.50 parts by weight of spherical powder and 22.50 parts by weight of flaky powder to make 100 parts by weight of silver powder. These were kneaded with a three-roll mill to prepare silver pastes of Samples 1 to 8, respectively.
得られた試料１〜８の各銀ペーストについて、２５℃における粘度をブルックフィールド社製粘度計（モデルＨＢＴ）にて測定した。得られた結果を、各銀ペーストの配合割合と共に、下記表１に示す。尚、粘度は、ずり速度が４／秒のときの値である。 About each obtained silver paste of samples 1-8, the viscosity in 25 degreeC was measured with the Brookfield viscometer (model HBT). The obtained results are shown in Table 1 below together with the blending ratio of each silver paste. The viscosity is a value when the shear rate is 4 / sec.
表１から明らかなように、本発明例である試料１〜５の銀ペーストの粘度は、スクリーン印刷に適した粘度である５０〜２００Ｐａ・ｓの範囲に入っていることが分る。一方、オレイン酸を含まない比較例の試料６〜７の銀ペーストは粘度が２００Ｐａ・ｓを越えてしまい、またオレイン酸の配合量が多い比較例の試料８の銀ペーストでは粘度が低くなり過ぎるため、いずれもスクリーン印刷に適さない。 As is apparent from Table 1, it can be seen that the silver pastes of Samples 1 to 5 which are examples of the present invention have a viscosity within the range of 50 to 200 Pa · s, which is a viscosity suitable for screen printing. On the other hand, the silver pastes of comparative samples 6 to 7 containing no oleic acid have a viscosity exceeding 200 Pa · s, and the silver paste of comparative sample 8 having a large amount of oleic acid is too low in viscosity. Therefore, neither is suitable for screen printing.
実際に、本発明例の試料１〜５の銀ペーストを、アルミナ基板上に幅０.６ｍｍ×長さ６０.０ｍｍのパタ−ンでスクリーン印刷したところ、微細なパターンを支障なく印刷することができた。また、得られたパターンは欠けや潰れがなく、良好な状態であった。しかし、比較例の試料６〜８の銀ペーストでは、版抜けが悪かったりパターンが滲んだりして、良好なスクリーン印刷は難しかった。 Actually, when the silver pastes of Samples 1 to 5 of the present invention were screen-printed on an alumina substrate with a pattern of width 0.6 mm × length 60.0 mm, a fine pattern could be printed without hindrance. did it. Further, the obtained pattern was in a good state with no chipping or crushing. However, in the silver pastes of Samples 6 to 8 of the comparative example, it was difficult to perform good screen printing because the plate omission was bad or the pattern was blurred.
次に、本発明例の試料１〜５の各銀ペーストについて、はんだ付け性評価した。即ち、アルミナ基板上に１０ｍｍ角のパターンでスクリーン印刷し、２００℃のオ−ブン中に３０分間放置して銀ペーストを硬化させた。その後、得られた銀ペースト硬化膜上にフラックスを塗布し、直径４.０ｍｍ及び高さ１.０ｍｍのはんだディスク（組成：Ｓｎ−３重量％Ａｇ−０.５重量％Ｃｕ）を載せ、２７０℃に加熱してはんだを溶融させ、はんだが溶融してから５秒後に冷却した。はんだは銀ペースト硬化膜上で拡がり、はんだ付け性が良好であることが分った。 Next, solderability was evaluated about each silver paste of the samples 1-5 of this invention example. That is, a 10 mm square pattern was screen-printed on an alumina substrate and left in a 200 ° C. oven for 30 minutes to cure the silver paste. Thereafter, a flux was applied onto the obtained cured silver paste film, and a solder disk (composition: Sn-3 wt% Ag-0.5 wt% Cu) having a diameter of 4.0 mm and a height of 1.0 mm was placed thereon. The solder was melted by heating to ° C., and cooled 5 seconds after the solder melted. It was found that the solder spreads on the cured silver paste film and the solderability is good.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103000252A (en) * | 2012-11-10 | 2013-03-27 | 江苏瑞德新能源科技有限公司 | Solar cell silver-backed slurry ultralow in silver content |
| JP2013196954A (en) * | 2012-03-21 | 2013-09-30 | Kyoto Elex Kk | Thermosetting conductive paste composition |
| JP2013196953A (en) * | 2012-03-21 | 2013-09-30 | Kyoto Elex Kk | Thermosetting conductive paste composition |
| WO2016124376A1 (en) * | 2015-02-02 | 2016-08-11 | Siemens Aktiengesellschaft | Sinterable mixture for binding components as well as composite and product therefrom |
| US9981859B2 (en) | 2013-10-29 | 2018-05-29 | Nichia Corporation | Positive electrode composition for non-aqueous electrolyte secondary battery and method of manufacturing thereof |
-
2008
- 2008-08-26 JP JP2008216559A patent/JP2010055788A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013196954A (en) * | 2012-03-21 | 2013-09-30 | Kyoto Elex Kk | Thermosetting conductive paste composition |
| JP2013196953A (en) * | 2012-03-21 | 2013-09-30 | Kyoto Elex Kk | Thermosetting conductive paste composition |
| CN103000252A (en) * | 2012-11-10 | 2013-03-27 | 江苏瑞德新能源科技有限公司 | Solar cell silver-backed slurry ultralow in silver content |
| US9981859B2 (en) | 2013-10-29 | 2018-05-29 | Nichia Corporation | Positive electrode composition for non-aqueous electrolyte secondary battery and method of manufacturing thereof |
| WO2016124376A1 (en) * | 2015-02-02 | 2016-08-11 | Siemens Aktiengesellschaft | Sinterable mixture for binding components as well as composite and product therefrom |
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