JPH04117434A - Production of laminate - Google Patents
Production of laminateInfo
- Publication number
- JPH04117434A JPH04117434A JP23578190A JP23578190A JPH04117434A JP H04117434 A JPH04117434 A JP H04117434A JP 23578190 A JP23578190 A JP 23578190A JP 23578190 A JP23578190 A JP 23578190A JP H04117434 A JPH04117434 A JP H04117434A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- laminate
- equivalent
- pressure
- varnish
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000003822 epoxy resin Substances 0.000 claims abstract description 22
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 22
- QGBSISYHAICWAH-UHFFFAOYSA-N dicyandiamide Chemical compound NC(N)=NC#N QGBSISYHAICWAH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002966 varnish Substances 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 17
- 238000010521 absorption reaction Methods 0.000 abstract description 12
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 8
- 239000003054 catalyst Substances 0.000 abstract description 8
- 230000006866 deterioration Effects 0.000 abstract description 5
- 238000009413 insulation Methods 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 230000005012 migration Effects 0.000 abstract description 4
- 238000000465 moulding Methods 0.000 abstract 2
- SSUJUUNLZQVZMO-UHFFFAOYSA-N 1,2,3,4,8,9,10,10a-octahydropyrimido[1,2-a]azepine Chemical compound C1CCC=CN2CCCNC21 SSUJUUNLZQVZMO-UHFFFAOYSA-N 0.000 abstract 1
- 239000004841 bisphenol A epoxy resin Substances 0.000 abstract 1
- 238000010030 laminating Methods 0.000 abstract 1
- 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 8
- 239000003795 chemical substances by application Substances 0.000 description 7
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 6
- 239000011889 copper foil Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 238000005476 soldering Methods 0.000 description 3
- MQJKPEGWNLWLTK-UHFFFAOYSA-N Dapsone Chemical compound C1=CC(N)=CC=C1S(=O)(=O)C1=CC=C(N)C=C1 MQJKPEGWNLWLTK-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- OHPBKUJGDFXDRM-UHFFFAOYSA-N 3,4-diethyl-5-(2-phenylpropan-2-yl)benzene-1,2-diamine Chemical compound CCC1=C(N)C(N)=CC(C(C)(C)C=2C=CC=CC=2)=C1CC OHPBKUJGDFXDRM-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 description 1
- ULKLGIFJWFIQFF-UHFFFAOYSA-N 5K8XI641G3 Chemical compound CCC1=NC=C(C)N1 ULKLGIFJWFIQFF-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- ILUISWOFWLEDTG-UHFFFAOYSA-N N,N-dichloro-1,1-diphenylmethanamine Chemical compound ClN(Cl)C(C1=CC=CC=C1)C1=CC=CC=C1 ILUISWOFWLEDTG-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 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 1
- 210000001161 mammalian embryo Anatomy 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229920003986 novolac Polymers 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Landscapes
- Reinforced Plastic Materials (AREA)
- Laminated Bodies (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、吸湿や吸水処理を行なった後の絶縁劣化や銅
マイグレーションの優れた印刷回路用基板に関するもの
である。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a printed circuit board that is excellent in insulation deterioration and copper migration after moisture absorption and water absorption treatment.
従来、基板の吸湿や吸水による絶縁劣化の防止のために
、ジシアンジアミンを硬化剤とする場合、吸水率の減少
のためにはエポキシ樹脂に対して１当量以下て使用する
のかよく、更に少量のジンアンジアミド使用（例えば、
０．３〜０．５当量）の方が吸水率の点てよいことがわ
かっている。Conventionally, when using dicyandiamine as a curing agent to prevent insulation deterioration due to moisture absorption and water absorption of the substrate, it is recommended to use less than 1 equivalent to the epoxy resin in order to reduce the water absorption rate, and even smaller amounts are used. use of diandiamide (e.g.
0.3 to 0.5 equivalent) is known to have a better water absorption rate.
本発明は、積層板用の硬化剤として広く用いられている
ジシアンジアミドを用いながら、基板を吸湿処理を行な
った時に発生する絶縁劣化及びそれらが主原因となる銅
マイグレーンヨンによる絶縁破壊が起こりに（い積層板
を提供するにある。The present invention uses dicyandiamide, which is widely used as a curing agent for laminates, but prevents insulation deterioration that occurs when substrates are subjected to moisture absorption treatment and insulation breakdown due to copper migration, which is the main cause of these deteriorations. (This is to provide a laminate board.)
本発明は、エポキシ樹脂ワニスを含浸して得たプリプレ
グを１枚もしくは複数枚重ね、これを金属鏡面板間に挟
み加熱加圧成形する積層板の製造方法において、
■ ビスフェノールＡ型エポキシ樹脂を５０重量％以上
含有するエポキシ樹脂、
■ 前記エポキシ樹脂１当量に対し、０．３〜０．７当
量のジシアンジアミド、及び
■ 硬化触媒として、１．８−ジアゾルビシクロ−（５
，４，０’）−ウンデセン〜７ （ＤＢＵ）を
必須成分として含有することを特徴とする積層板の製造
方法を要旨とするものである。The present invention provides a method for producing a laminate in which one or more prepregs impregnated with an epoxy resin varnish are stacked, sandwiched between metal mirror plates, and then heated and pressure-molded. an epoxy resin containing at least % by weight, (1) dicyandiamide in an amount of 0.3 to 0.7 equivalents per equivalent of the epoxy resin, and (2) 1.8-diazolbicyclo-(5
, 4,0')-undecene~7 (DBU) as an essential component.
本発明に使用するエポキシ樹脂は、ビスフェノールＡ型
エポキシ樹脂を５０重量％以上含むものである。全量ビ
スフェノールＡ型エポキシ樹脂を使用してもよいし、耐
熱性も向上させるためにノボラック型エポキシ樹脂系の
他のタイプのものを５０重量％以下使用してもよい。ビ
スフェノールＡ型エポキシ樹脂が５０重量％未満の場合
は、耐熱性は一般的には向上するものの、硬くもろくな
り、銅箔との接着力も低下してくる。ビスフェノールＡ
型エポキシ樹脂の配合割合は７０重量％以上か好ましい
。The epoxy resin used in the present invention contains 50% by weight or more of bisphenol A type epoxy resin. The entire amount of bisphenol A type epoxy resin may be used, or in order to improve heat resistance, other types of novolac type epoxy resins may be used in an amount of 50% by weight or less. When the bisphenol A type epoxy resin is less than 50% by weight, the heat resistance is generally improved, but it becomes hard and brittle, and the adhesive strength with copper foil is also reduced. Bisphenol A
The blending ratio of the mold epoxy resin is preferably 70% by weight or more.
本発明に使用する硬化剤は、ジシアンジアミドである。The curing agent used in the present invention is dicyandiamide.
ジシアンジアミドは、硬化触媒ＤＢＵを併用するのて、
エポキシ樹脂１当量に対し、０．３〜０．７当量である
。０．３当量未満ては成形性か悪く、ガラス移転点や接
着性か劣り、硬化促進のために触媒を多く使用すると、
耐熱性なとが低下するようになる。一方、０．７当量よ
り大きくすると、硬化性は良好となるか、吸水による電
気特性の劣化が大きくなってくる。好ましくは０．４〜
０．６当量である。硬化剤はジンアンジアミド以外のも
のを併用することも可能である。併用しうる硬化剤は芳
香族アミン系のものが好ましく、ジアミノジフェニルメ
タン（ＤＤＭ） 、ジクロルンアミノジフェニルメタン
（ＤＤＤＭ） 、ジアミノジフェニルスルホン（ＤＤＳ
） 、ジアミノジエチルジメチルジフェニルメタン（キ
ュアハード■）、ジアミノジフェニルエーテル（ＤＤＥ
）などを挙げることかてきる。かかる硬化剤の量はエポ
キシ樹脂１当量に対して０．３当量以下が好ましい。Since dicyandiamide is used together with the curing catalyst DBU,
The amount is 0.3 to 0.7 equivalent per equivalent of epoxy resin. If the amount is less than 0.3 equivalent, the moldability will be poor, the glass transition point and adhesiveness will be poor, and if a large amount of catalyst is used to accelerate curing,
Heat resistance decreases. On the other hand, if the amount is larger than 0.7 equivalent, the curability will be good or the electrical properties will deteriorate significantly due to water absorption. Preferably 0.4~
It is 0.6 equivalent. It is also possible to use a curing agent other than diandiamide in combination. The curing agents that can be used in combination are preferably those based on aromatic amines, such as diaminodiphenylmethane (DDM), dichloraminodiphenylmethane (DDDM), and diaminodiphenyl sulfone (DDS).
), Diaminodiethyldimethyldiphenylmethane (Cure Hard ■), Diaminodiphenyl ether (DDE
), etc. The amount of such curing agent is preferably 0.3 equivalent or less per equivalent of epoxy resin.
本発明においては、硬化剤ジシアンジアミドと共に硬化
触媒としてＤＢＵを使用することに特徴かある。ジシア
ンジアミドにＤＢＵを併用すると、通常の硬化触媒イミ
ダゾール系のものに比べて、得られた積層板からのイオ
ン抽出水の導電率か小さい。即ち、積層板中の遊離又は
加水分解性イオンが少ないことが見出された。The present invention is characterized by the use of DBU as a curing catalyst together with the curing agent dicyandiamide. When DBU is used in combination with dicyandiamide, the conductivity of the ion-extracted water from the resulting laminate is lower than that of a typical imidazole-based curing catalyst. That is, it was found that there were fewer free or hydrolyzable ions in the laminate.
イミダゾール系硬化触媒を使用した場合、積層板から抽
出された抽出水中には、クロム、ブロム、酢酸、ギ酸等
の陰イオン、及びアンモニウム、ナトリウム等の陽イオ
ンが存在するが、ＤＢＵを硬化触媒とした場合、これら
のイオンの抽出量が非常に／ｈさくなり、抽出水の導電
率が小さくなる。When an imidazole-based curing catalyst is used, anions such as chromium, bromine, acetic acid, and formic acid, and cations such as ammonium and sodium are present in the extracted water extracted from the laminate. In this case, the amount of these ions extracted per hour becomes very small, and the conductivity of the extracted water becomes small.
ＤＢＵの配合量は、エポキシ樹脂に対して０．０４〜０
．２重量％か好ましい。The blending amount of DBU is 0.04 to 0 relative to the epoxy resin.
．． 2% by weight is preferred.
０．０４重量％未満ては硬化促進効果が小さく、０、２
重量％より多いと、耐熱性、接着性に問題がでてくる可
能性がある。If it is less than 0.04% by weight, the curing accelerating effect is small;
If the amount exceeds % by weight, problems may arise in heat resistance and adhesiveness.
第１表に示す配合にてエポキシ樹脂ワニスを調製した。 Epoxy resin varnishes were prepared according to the formulations shown in Table 1.
エポキシ樹脂はエポキシ当量の５００のビこのワニスを
ガラスクロスに含浸してプリプレグを得、この複数枚と
その両面に銅箔を重ね合わせて常法により、加熱加圧成
形し、厚さ１，６胚の両面鋼張積層板を得た。The epoxy resin is made by impregnating glass cloth with a vinyl varnish having an epoxy equivalent of 500 to obtain a prepreg, which is then laminated with copper foil on both sides and molded under heat and pressure in a conventional manner to a thickness of 1.6 mm. A double-sided steel-clad laminate of the embryo was obtained.
得られた積層板の形成状及び特性を調へ、第１表に示す
結果を得た。The formed shape and characteristics of the obtained laminate were examined, and the results shown in Table 1 were obtained.
測定方法は次の通りである。The measurement method is as follows.
（ｉ）抽出水の導電率（目標３５０以下）銅箔をエツチ
ングで除去し、表面を洗浄した後、３ｇを試料として採
り、水３０ｇを加えプレッシャークツカー処理を４８時
間行った。その後得られた抽出水の導電率を求めた。(i) Electrical conductivity of extracted water (target 350 or less) After removing the copper foil by etching and washing the surface, 3 g was taken as a sample, 30 g of water was added, and pressure cooker treatment was performed for 48 hours. Thereafter, the conductivity of the extracted water was determined.
（ｉｉ）吸水率の半田耐熱性
プレッシャークツカー処理（１２５°Ｃ１２，３気圧）
を１時間行った試料につき、２８０°Ｃて６０秒間半田
溶に浸し、ふくれの有無をみた。(ii) Water absorption rate soldering heat resistance pressure couture treatment (125°C, 12,3 atm)
The samples that had been subjected to this process for one hour were immersed in solder melt for 60 seconds at 280°C, and the presence or absence of blisters was examined.
○：以上なし △：ふくれ発生
×：ふくれ多発
（ｉｉ）成形性
銅箔をエツチングて除去した後、積層板表面外観を目視
て観察し、ボイドの有無により成形性を判定した。○: None. Δ: Occurrence of blistering. ×: Frequent blistering. (ii) Formability After etching and removing the copper foil, the surface appearance of the laminate was visually observed, and formability was determined based on the presence or absence of voids.
Ｏ：ボイドなし △：ボイドあり
各実施例で得られた積層板はプレッシャークツカー処理
後の抽出水の導電率が小さく、吸水後の半田耐熱性及び
体積抵抗率も良好である。これらはＤＢＵを硬化触媒と
して使用しているか、比較例１〜３の２エチル４メチル
イミダゾールを硬化触媒とした場合に比較して、それら
の特性は同等以上である。O: No voids △: With voids The laminates obtained in each example have low conductivity of extracted water after pressure-packing treatment, and good soldering heat resistance and volume resistivity after water absorption. These properties are equivalent to or better than those using DBU as a curing catalyst or when 2-ethyl-4-methylimidazole of Comparative Examples 1 to 3 is used as a curing catalyst.
比較例４．５はジシアンジアミドの量か適量ではないの
で、一部の特性か劣ったものとなっている。In Comparative Examples 4.5, the amount of dicyandiamide was not appropriate, so some of the properties were inferior.
以上の結果からも明らかなように、本発明により得られ
た積層板は、プレッシャークツカー抽出水の導電率か小
さく、吸水半田耐熱性もすぐれている。従って、銅マイ
グレーションも生じ難い。As is clear from the above results, the laminate obtained by the present invention has a low conductivity of water extracted from a pressure cooker and excellent water absorption and soldering heat resistance. Therefore, copper migration is also less likely to occur.
成形性も良好であり、その他の緒特性も特に問題ないの
て、過酷な条件で処理され、使用される印刷回路用基板
として使用されるのに適している。It has good moldability and has no particular problems with other mechanical properties, so it is suitable for use as printed circuit boards that are processed and used under harsh conditions.
Claims (1)
１枚もしくは複数枚重ね、これを金属鏡面板間に挟み加
熱加圧成形する積層板の製造方法において、 〔１〕ビスフェノールＡ型エポキシ樹脂を５０重量％以
上含有するエポキシ樹脂、 〔２〕前記エポキシ樹脂１当量に対し、０．３〜０．７
当量のジシアンジアミド、及び 〔３〕硬化触媒として、１，８−ジアゾ−ビシクロー（
５，４，０）−ウンデセン−７（ＤＢＵ）を 必須成分として含有することを特徴とする積層板の製造
方法。(1) A method for manufacturing a laminate in which one or more prepregs impregnated with an epoxy resin varnish are stacked, sandwiched between metal mirror plates, and then heated and pressure-molded. Epoxy resin containing 50% by weight or more, [2] 0.3 to 0.7 per equivalent of the epoxy resin
an equivalent amount of dicyandiamide, and [3] 1,8-diazo-bicyclo(
A method for producing a laminate, characterized in that it contains 5,4,0)-undecene-7 (DBU) as an essential component.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23578190A JPH04117434A (en) | 1990-09-07 | 1990-09-07 | Production of laminate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23578190A JPH04117434A (en) | 1990-09-07 | 1990-09-07 | Production of laminate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04117434A true JPH04117434A (en) | 1992-04-17 |
Family
ID=16991149
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23578190A Pending JPH04117434A (en) | 1990-09-07 | 1990-09-07 | Production of laminate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04117434A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019535886A (en) * | 2016-10-28 | 2019-12-12 | ライヒホールド アクティーゼルスカブ | Rapid curing epoxy resin composition for fiber-matrix semi-finished products |
-
1990
- 1990-09-07 JP JP23578190A patent/JPH04117434A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019535886A (en) * | 2016-10-28 | 2019-12-12 | ライヒホールド アクティーゼルスカブ | Rapid curing epoxy resin composition for fiber-matrix semi-finished products |
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