JPH0485339A - Preparation of epoxy resin laminate - Google Patents
Preparation of epoxy resin laminateInfo
- Publication number
- JPH0485339A JPH0485339A JP19926690A JP19926690A JPH0485339A JP H0485339 A JPH0485339 A JP H0485339A JP 19926690 A JP19926690 A JP 19926690A JP 19926690 A JP19926690 A JP 19926690A JP H0485339 A JPH0485339 A JP H0485339A
- Authority
- JP
- Japan
- Prior art keywords
- epoxy resin
- laminate
- epoxy
- equivalent
- resin
- 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
- 239000003822 epoxy resin Substances 0.000 title claims abstract description 30
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 30
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 18
- 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 9
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- 239000002184 metal Substances 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000004593 Epoxy Substances 0.000 claims description 12
- 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 claims description 10
- 229920005989 resin Polymers 0.000 claims description 9
- 239000011347 resin Substances 0.000 claims description 9
- 229920003986 novolac Polymers 0.000 claims 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 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract description 9
- 239000012535 impurity Substances 0.000 abstract description 5
- 229910052802 copper Inorganic materials 0.000 abstract description 4
- 239000010949 copper Substances 0.000 abstract description 4
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 238000003825 pressing Methods 0.000 abstract 2
- 238000010521 absorption reaction Methods 0.000 description 9
- 239000011889 copper foil Substances 0.000 description 5
- 230000006866 deterioration Effects 0.000 description 4
- 239000011521 glass Substances 0.000 description 3
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- BDPMIHVEHJUJIW-UHFFFAOYSA-N (2,3-dichlorophenyl)-phenylmethanediamine Chemical compound C=1C=CC(Cl)=C(Cl)C=1C(N)(N)C1=CC=CC=C1 BDPMIHVEHJUJIW-UHFFFAOYSA-N 0.000 description 2
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005530 etching Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 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
- 230000005856 abnormality Effects 0.000 description 1
- 150000008065 acid anhydrides Chemical class 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004982 aromatic amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010411 cooking Methods 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000000691 measurement method Methods 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 229910000679 solder Inorganic materials 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/03—Use of materials for the substrate
- H05K1/0313—Organic insulating material
- H05K1/032—Organic insulating material consisting of one material
- H05K1/0326—Organic insulating material consisting of one material containing O
Landscapes
- Reinforced Plastic Materials (AREA)
- Epoxy Resins (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は、吸湿又は吸水処理を行った場合の絶縁劣化が
少ない印刷回路用基板に関するものである。DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a printed circuit board that exhibits little insulation deterioration when subjected to moisture absorption or water absorption treatment.
（従来の技術）
従来、・エポキシ樹脂ガラス基材印刷回路基板は吸湿や
吸水による絶縁劣化を防止するために、硬化剤としてジ
シアンジアミド以外のアミン系°硬化剤を使用する、ジ
シアンジアミドを使用する場合でも１当量以下、通常は
０．６〜０．７当量程度をする、あるいはガラス基材の
表面処理剤としてアミノシラン系カップリング剤を使用
すること等がある。また、エポキシ樹脂中のＣＩ−、Ｓ
Ｏ４’−、Ｎａ“イオン量を極力少なくすることも効果
的である。(Prior art) Conventionally, epoxy resin glass-based printed circuit boards use amine-based curing agents other than dicyandiamide as hardening agents to prevent insulation deterioration due to moisture absorption and water absorption. Even when dicyandiamide is used, The amount may be 1 equivalent or less, usually about 0.6 to 0.7 equivalents, or an aminosilane coupling agent may be used as a surface treatment agent for the glass substrate. In addition, CI-, S in epoxy resin
It is also effective to reduce the amount of O4'- and Na' ions as much as possible.
（発明が解決しようとする課題）
本発明は、吸湿や吸水による絶縁劣化を防止するため、
前記従来の技術を考慮に入れながら、それよりも効果の
ある方法を種々検討して完成されたものであり、耐水耐
湿性が良好であり、銅マイグレーションの防止にも効果
的な積層板の製造方法を提供するものである。(Problems to be Solved by the Invention) The present invention aims to prevent insulation deterioration due to moisture absorption and water absorption.
This was completed by taking into account the above-mentioned conventional technology and examining various methods that were more effective than the conventional technology, and produced a laminate that has good water and moisture resistance and is effective in preventing copper migration. The present invention provides a method.
（課題を解決するための手段）
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、これを金属鏡面板に挟み
加熱加圧する積層板の製造方法において、
エポキシ樹脂ワニスとして、
（ａｌ エポキシ樹脂 １当量 及び（ｂｌ 硬化
剤 ０．１５〜０．５０当量からなり、硬化剤の
うち、５０重量％以上で、かつエポキシ樹脂に対し０．
１５当量以上かジシアンジアミドであることを特徴とす
るエポキシ樹脂積層板の製造方法である。(Means for Solving the Problems) The present invention provides a method for manufacturing a laminate in which one or more prepregs impregnated with epoxy resin varnish are stacked, sandwiched between metal mirror plates, and heated and pressed. The varnish is composed of (al: 1 equivalent of epoxy resin) and (bl: 0.15 to 0.50 equivalents of curing agent, with the amount of the curing agent being 50% by weight or more and 0.0% by weight relative to the epoxy resin.
This is a method for producing an epoxy resin laminate, characterized in that the dicyandiamide has an equivalent weight of 15 or more.
本発明において用いられる硬化剤はジシアンジアミドを
主成分とするか、他の硬化剤としては、ジアミノジフェ
ニルメタン（ＤＤＭ） 、ジクロルジアミノジフェニル
メタン（ＤＤＤＭ）、ジアミノジフェニルスルフォン
アミノ−３，３゛−ジエチル−５．５“−ジメチルジフ
ェニルメタン（キュアハード■）、水素添加ジアミノジ
フェニルメタン、ジアミノジフェニルエーテル（ＤＤＥ
）等の芳香族アミン系硬化剤を挙げることかできる。酸
無水物等も使用することかできるが、物理特性、特に半
田処理による銅箔接着強度の劣化か大きく、避ける方か
好ましい。The curing agent used in the present invention is mainly composed of dicyandiamide, or other curing agents include diaminodiphenylmethane (DDM), dichlorodiaminodiphenylmethane (DDDM), diaminodiphenylsulfonamino-3,3'-diethyl-5 .5"-dimethyldiphenylmethane (Cure Hard ■), hydrogenated diaminodiphenylmethane, diaminodiphenyl ether (DDE
) and the like can be mentioned. Although acid anhydrides and the like can be used, it is preferable to avoid them because the physical properties, especially the copper foil adhesive strength due to soldering, are significantly deteriorated.
エポキシ樹脂に対する硬化剤の当量は、通常の場合より
低く０．１５〜０．５０とし、主成分としてジシアンジ
アミドを使用する。この硬化剤当量が０．１５以下では
硬化か遅く、また十分に硬化しない。硬化を速めるため
にイミダゾール等の触媒量を多くすると、成形性か悪く
なり、積層板の色調も濃くなってしまう。一方０．５０
以上となると、硬化性はよいが、吸水による電気特性の
劣化が大きくなる。The equivalent weight of the curing agent to the epoxy resin is set to 0.15 to 0.50, which is lower than usual, and dicyandiamide is used as the main component. If the curing agent equivalent is less than 0.15, curing will be slow and will not be curing sufficiently. If the amount of catalyst such as imidazole is increased in order to speed up curing, the moldability will deteriorate and the color tone of the laminate will become darker. On the other hand, 0.50
If it is above, the curing property is good, but the deterioration of the electrical properties due to water absorption becomes large.
ジシアンジアミドの量は０．１５当量以上で、かつ全硬
化剤量の５０重量％以上とすることにより、良好な硬化
性を有し、接着性も良好で、他の積層板特性もよい。こ
のような硬化剤配合により概ね良好な特性の積層板を得
ることができる。When the amount of dicyandiamide is 0.15 equivalent or more and 50% by weight or more of the total amount of curing agent, good curability, good adhesion, and other laminate properties are obtained. By blending the curing agent in this manner, a laminate with generally good properties can be obtained.
次に、エポキシ樹脂の配合について説明する。Next, the formulation of the epoxy resin will be explained.
エポキシ樹脂の中て、ビスフェノールＡ型エポキシ樹脂
を６５〜９３重量％使用し、残りはエポキシノボラック
樹脂を使用するのが好ましい。It is preferable to use 65 to 93% by weight of bisphenol A type epoxy resin among the epoxy resins, and use epoxy novolak resin for the remainder.
エポキシ樹脂としてエポキシノボラック樹脂を併用する
ことにより架橋密度が高くなり、耐熱性が向上する。全
エポキシ樹脂中エポキシノボラック樹脂が３５％以上で
は硬化物の硬度が高くなりすぎ、もろくなる。また７％
以下では耐熱性向上効果・が小さい。By using an epoxy novolak resin as the epoxy resin, the crosslinking density increases and heat resistance improves. If the epoxy novolak resin in the total epoxy resin is 35% or more, the hardness of the cured product becomes too high and becomes brittle. Another 7%
Below this, the effect of improving heat resistance is small.
また、このビスフェノールＡ型エポキシ樹脂は２種以上
使用する場合、そのうちの最も多く使用しているエポキ
シ樹脂とのエポキシ当量の比が１。In addition, when two or more types of bisphenol A type epoxy resins are used, the epoxy equivalent ratio with the epoxy resin used most often is 1.
５以上であるエポキシ樹脂の合計がビスフェノールＡ型
エポキシ樹脂全量に対して６０重量％以下とするのか好
ましい。It is preferable that the total amount of epoxy resins of 5 or more is 60% by weight or less based on the total amount of bisphenol A epoxy resin.
このような配合とすることにより、樹脂と硬化剤の調和
かとれ、より良好な特性の積層板が得られる。By using such a blend, the resin and the curing agent can be harmonized, and a laminate with better properties can be obtained.
硬化剤のジシアンジアミドは汎用性かあり、物理特性、
電気特性がバランスよ＜、Ｎａ’ 、Ｃｌ−などのイオ
ン性不純物も樹脂配合、硬化剤の種類及び量を適切に選
べば、非常に少な（なり、吸水特性の向上に有益である
。The curing agent dicyandiamide is versatile, has physical properties,
If the electrical properties are well-balanced, ionic impurities such as Na' and Cl- can be reduced to a very small amount if the resin composition and the type and amount of the curing agent are appropriately selected, which is beneficial for improving the water absorption properties.
また、併用する芳香族系アミン硬化剤及びエポキシノボ
ラック樹脂もイオン性不純物が比較的少なく、これらの
点も、積層板特性か良好なものとなる大きな理由である
。Furthermore, the aromatic amine curing agent and epoxy novolac resin used in combination also have relatively few ionic impurities, and these points are also a major reason why the laminate has good properties.
（実施例） 以下、実施例及び比較例により本発明を説明する。(Example) The present invention will be explained below with reference to Examples and Comparative Examples.
第１表に示す配合物で溶剤に溶解し、樹脂分約５０重量
％のワニスを調製した。このワニスをガラスクロスに含
浸し、乾燥しプリプレグを得、このプリプレグの複数枚
とその両面に銅箔を重ね合わせ、常法によ・り加熱加圧
成形して厚さ１．６ｎｏの両面銅張積層板を得た。The formulations shown in Table 1 were dissolved in a solvent to prepare a varnish having a resin content of about 50% by weight. A glass cloth is impregnated with this varnish, dried to obtain a prepreg, multiple sheets of this prepreg and copper foil are layered on both sides, and the double-sided copper foil is molded under heat and pressure in a conventional manner to a thickness of 1.6 mm. A stretched laminate was obtained.
上記プリプレグ及び積層板について、第１表ζこ示す特
性を測定した。The properties shown in Table 1 were measured for the above prepreg and laminate.
測定方法は以下の通りである。The measurement method is as follows.
（ｉ）耐熱性（ガラス転移点）
粘弾性試験機により、昇温速度３℃／分とし、Ｔａｎδ
のピークにより求めた。(i) Heat resistance (glass transition point) Tanδ
It was determined by the peak of
（ｉｉ）吸水率の半田耐熱性
プレッシャクッ力処理（１２５°Ｃ１２，３気圧）を１
時間行った試料につき、２８０℃で６０秒間半田浴に侵
し、ふくれの有無をみた。(ii) Water absorption rate of soldering heat resistance pressure-cooking force treatment (125°C, 12,3 atm)
The samples that had been used for several hours were immersed in a solder bath at 280° C. for 60 seconds, and the presence or absence of blisters was observed.
○：異常なし △：ふくれ発生
（ｉｉｉ）プリプレグの保存性
２０℃で３０日間保存後、１７０℃でのゲル化時間を測
定した。（初期値を１００％として）０２９０％以上
○：６０〜８９％ ×、５９％以下（ｉｖ）成形性
銅箔をエツチングで除去した後、積層板表面外観を目視
で観察した。○: No abnormality △: Blistering (iii) Storage property of prepreg After storage at 20°C for 30 days, gelation time at 170°C was measured. (assuming the initial value is 100%) 0290% or more
○: 60 to 89% ×, 59% or less (iv) Formability After removing the copper foil by etching, the surface appearance of the laminate was visually observed.
（Ｖ）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、４ｇを試料とし
て採り、水２００ｇを加えプレソシャクッ力処理を４８
時間行った。その後得られた抽出水の導電率を求めた。(V) Electrical conductivity of extracted water (target 350 or less) After removing the copper foil by etching and cleaning the surface, take 4 g as a sample, add 200 g of water, and apply pre-soaking force treatment for 48 hours.
Time went. Thereafter, the conductivity of the extracted water was determined.
第１表の結果をみると、各実施例はすべての特性におい
て良好である。特にエポキシノボラック樹脂の併用、エ
ポキシ当量の異なる２種のビスフェノールＡ型エポキシ
樹脂の使用により、耐熱性が向上するか、エポキシ当量
の異なるものの多量の配合はイオン性不純物の低下には
よくないものとなる。Looking at the results in Table 1, each example is good in all characteristics. In particular, heat resistance can be improved by using epoxy novolac resin in combination or two types of bisphenol A epoxy resins with different epoxy equivalents, or blending large amounts of different epoxy equivalents is not good for reducing ionic impurities. Become.
（発明の効果）
以上の実施例なとからも明らかなように、本発明により
得られたエポキシ樹脂積層板は、全体として調和のとれ
たすぐれた特性を有しており、耐水耐湿性がすぐれてお
り、イオン性不純物か少ないことにより銅マイグレーシ
ョンも発生し難くなる。実施例におけるエポキシノボラ
ック樹脂の併用、あるいは２種のビスフェノールＡ型エ
ポキシ樹脂の使用では、低分子量のものを少量加えた場
合、耐熱性か更に向上する。(Effects of the Invention) As is clear from the examples above, the epoxy resin laminate obtained by the present invention has well-balanced and excellent characteristics as a whole, and has excellent water and moisture resistance. Since there are fewer ionic impurities, copper migration is also less likely to occur. In the combined use of epoxy novolac resins or the use of two types of bisphenol A type epoxy resins in the examples, when a small amount of a low molecular weight resin is added, the heat resistance is further improved.
Claims (3)
１枚もしくは複数枚重ね、これを金属鏡面板に挟み加熱
加圧する積層板の製造方法において、エポキシ樹脂ワニ
スとして、（ａ）エポキシ樹脂１当量及び （ｂ）硬化剤０．１５〜０．５０当量からなり、硬化剤
のうち、５０重量％以上でかつ０．１５当量以上がジシ
アンジアミドであることを特徴とするエポキシ樹脂積層
板の製造方法。(1) In a method for manufacturing a laminate in which one or more prepregs impregnated with an epoxy resin varnish are stacked and sandwiched between metal mirror plates and heated and pressed, the epoxy resin varnish includes: (a) 1 equivalent of the epoxy resin; and (b) a method for producing an epoxy resin laminate comprising 0.15 to 0.50 equivalents of a curing agent, wherein 50% by weight or more and 0.15 equivalents or more of the curing agent is dicyandiamide.
樹脂を６５〜９３重量％とエポキシノボラック樹脂３５
〜７重量％を使用することを特徴とする請求項１記載の
積層板の製造方法。(2) 65 to 93% by weight of bisphenol A type epoxy resin and 35% by weight of epoxy novolak resin as epoxy resin
2. The method for producing a laminate according to claim 1, characterized in that ~7% by weight is used.
場合において、そのうちの最も多く使用している樹脂と
のエポキシ当量の比（エポキシ当量の大きいもの対小さ
いものの比）が１．５以上であるエポキシ樹脂の合計が
ビスフェノールＡ型エポキシ樹脂全量に対し６０重量％
以下であることを特徴とする請求項１記載の積層板の製
造方法。(3) When two types of bisphenol A type epoxy resins are used, an epoxy resin whose epoxy equivalent ratio (ratio of large to small epoxy equivalent) with the resin used most frequently is 1.5 or more. The total amount of resin is 60% by weight based on the total amount of bisphenol A epoxy resin.
The method for manufacturing a laminate according to claim 1, characterized in that:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19926690A JPH0485339A (en) | 1990-07-30 | 1990-07-30 | Preparation of epoxy resin laminate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19926690A JPH0485339A (en) | 1990-07-30 | 1990-07-30 | Preparation of epoxy resin laminate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0485339A true JPH0485339A (en) | 1992-03-18 |
Family
ID=16404933
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19926690A Pending JPH0485339A (en) | 1990-07-30 | 1990-07-30 | Preparation of epoxy resin laminate |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0485339A (en) |
-
1990
- 1990-07-30 JP JP19926690A patent/JPH0485339A/en active Pending
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