JPS58189260A - Production of polyimide varnish - Google Patents
Production of polyimide varnishInfo
- Publication number
- JPS58189260A JPS58189260A JP7133382A JP7133382A JPS58189260A JP S58189260 A JPS58189260 A JP S58189260A JP 7133382 A JP7133382 A JP 7133382A JP 7133382 A JP7133382 A JP 7133382A JP S58189260 A JPS58189260 A JP S58189260A
- Authority
- JP
- Japan
- Prior art keywords
- polyimide
- powder
- varnish
- diamine
- acid anhydride
- 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.)
- Granted
Links
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
- Paints Or Removers (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
Abstract
Description
【発明の詳細な説明】
本発明は、耐熱性物質を与える新規なポリイミド粉末含
有ポリイミドワニスの製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a novel polyimide powder-containing polyimide varnish that provides a heat-resistant material.
従来、粉末含有ポリイミドワニスの製造方法としては2
通常のポリイミドワニスに、無機又は有機の粉末を入れ
、攪拌等の機械的方法により混合分散させるという方法
が取られていた。Conventionally, there are two methods for producing powder-containing polyimide varnish.
The conventional method has been to add inorganic or organic powder to ordinary polyimide varnish and mix and disperse it using mechanical methods such as stirring.
しかし、この方法では、ワニス中に粉末を大量、均一に
分散させることが困離であり、このワニ1−
スを顕微鏡下で観察すると多数の二次凝集体が見られる
。However, with this method, it is difficult to uniformly disperse a large amount of powder in the varnish, and when the varnish is observed under a microscope, a large number of secondary aggregates are seen.
このフェスをたとえばスクリーン印刷用インクとして使
用した場合、インクのスクリーンからの′“抜け″が悪
く、多数回印刷ができず、P4られだ塗、布膜も二次凝
集体が散見され、均一な塗布膜が侍られない。For example, when this face is used as an ink for screen printing, the ink does not easily escape from the screen, making it impossible to print multiple times. The coating film cannot be maintained.
本発明の目的は、粉末が大量、均一にワニス中に分散し
た。ポリイミドワニスの製造方法を提供することにある
。The object of the present invention is to disperse a large amount of powder uniformly in the varnish. An object of the present invention is to provide a method for producing polyimide varnish.
本発明は、上記目的を達成するため次の構成。The present invention has the following configuration to achieve the above object.
すなわち、テトラ有機カルボン酸無水物々ジアミンを溶
剤中で反応させ、得られたポリイミド前駆体溶液をイミ
ド閉環温度で加熱してポリイミド粉末を析出させ、得ら
れたポリイミド粉末の懸濁液中で、テトラ有機カルボン
酸無水物とジアミンを反応させポリイミド前駆体を形成
するポリイミドワニスの製造方法を特徴とするものであ
る。That is, a tetraorganic carboxylic acid anhydride diamine is reacted in a solvent, the obtained polyimide precursor solution is heated at the imide ring closing temperature to precipitate polyimide powder, and in the suspension of the obtained polyimide powder, The present invention is characterized by a method for producing a polyimide varnish, in which a tetraorganic carboxylic acid anhydride and a diamine are reacted to form a polyimide precursor.
本発明に適用されるテトラ有機カルボン酸無水物とけ、
一般式 OぐSg〕R1(g〕0で示されるもので、同
式のR4は、炭素数6以上20以下の芳香族環又は芳香
族性複素環で、カルボニル基がオルソ又はぺりの位置に
結合されるものである。R1の例としてはフェニル基、
ナフタレン基、ペリレン基。Tetra organic carboxylic acid anhydride solution applied to the present invention,
It is represented by the general formula OgSg]R1(g)0, and R4 in the same formula is an aromatic ring or aromatic heterocycle having 6 to 20 carbon atoms, and the carbonyl group is bonded to the ortho or peri position. Examples of R1 include phenyl group,
naphthalene group, perylene group.
ジフェニル基、ジフェニルエーテル基、ジフェニルスル
ホン基、2.2’−:/フェニルプロパン基、ベンゾフ
ェノン基表どが典型的な例として挙げられるが、これら
に限定されない。特に望ましいのはフェニル基とベンゾ
フェノン基でアル。Typical examples include, but are not limited to, a diphenyl group, a diphenyl ether group, a diphenylsulfone group, a 2.2'-:/phenylpropane group, and a benzophenone group. Particularly desirable are phenyl groups and benzophenone groups.
なお、粉末の原料として使用するテトラ有機カルボン酸
無水物とポリイミド粉末の顕濁液中でポリイミド前駆体
を形成するために使用するテトラ有機カルボン酸無水物
とは同一物でも異なった物質でもよい。The tetraorganic carboxylic acid anhydride used as a raw material for the powder and the tetraorganic carboxylic acid anhydride used to form the polyimide precursor in the polyimide powder suspension may be the same or different substances.
次に本発明に適用されるシア”ミンとは、一般式H2N
−R2−NH2で示されるもので、同式のR2は、芳香
族環又は芳香族性複素環から成るものである。Next, the cyamine applied to the present invention has the general formula H2N
It is represented by -R2-NH2, and R2 in the same formula consists of an aromatic ring or an aromatic heterocycle.
R2の例トしてジフェニルエーテル基、フェニル基。Examples of R2 include diphenyl ether group and phenyl group.
トルイレン基、ジフェニルメタン基、ジフェニルスルホ
ン基などが典型的な例として挙げられる。Typical examples include toluylene group, diphenylmethane group, and diphenylsulfone group.
=6−
壕だ、これらの基の粉末形性能、耐熱性に悪影響を与え
ない範囲で、これらの基がアミノ基、アシド基、カルボ
キシル基、スルホン酸基などの置換基を有していてもよ
い。とくにジフェニルエーテル基、フェニル基が望壕し
く用いられる。= 6- Yes, even if these groups have substituents such as amino groups, acid groups, carboxyl groups, sulfonic acid groups, etc., as long as they do not adversely affect the powder form performance and heat resistance of these groups. good. In particular, diphenyl ether groups and phenyl groups are preferably used.
なお、粉末の原料として使用されるジアミンとポリイミ
ド粉末の懸濁液中でポリイミド前駆体を形成するために
使用されるジアミンとは同一物でも異なった物質であっ
てもよい。Note that the diamine used as a raw material for the powder and the diamine used to form the polyimide precursor in the suspension of polyimide powder may be the same or different substances.
テトラ有機カルボン酸無水物とジアミンを反応させるた
めに用いる溶剤としてはポリマの溶解性の面から主とし
て極性溶媒が望ましい。極性溶媒の例として、ジメチル
スルホキシド、ジメチルホルムアミド、ジメチルアセト
アミド、N−メチル2−ピロリドン、ヘキサメチルホス
ホロアミドなどが好ましく用いられる。The solvent used for reacting the tetraorganic carboxylic acid anhydride and the diamine is preferably a polar solvent from the viewpoint of polymer solubility. As examples of polar solvents, dimethyl sulfoxide, dimethylformamide, dimethylacetamide, N-methyl 2-pyrrolidone, hexamethylphosphoramide, etc. are preferably used.
上記テトラ有機、、、カルボン酸無水物とジアミンを溶
剤中で反応させる方法としては溶剤中に攪拌下でジアミ
ンを添加して溶かし、溶解後テトラ有機カルボン酸無水
物を添加して反応させる。−勇非4−
誓一テトラ有機カルボン酸無水物(A)とジアミン(B
)との比(A> / (B)は、0.7〜1.好1しく
け08〜0.95が望ましい。この比が07以下では製
造されたフェノの展延性が悪く、スクリーン印刷用イン
クとして使用する際連続して印刷することが困難になる
。As a method for reacting the above tetraorganic carboxylic acid anhydride and diamine in a solvent, the diamine is added and dissolved in the solvent with stirring, and after dissolving, the tetraorganic carboxylic acid anhydride is added and reacted. -Yuhi 4- Seiichi tetra organic carboxylic acid anhydride (A) and diamine (B
) The ratio (A>/(B) is preferably 0.7 to 1.0, preferably 08 to 0.95. If this ratio is less than 07, the phenol produced will have poor malleability, making it difficult to use for screen printing. When used as ink, it becomes difficult to print continuously.
ポリイミド前駆体溶液でのポリイミド前駆体の濃度は2
0〜′55%好壕しくけ23〜30%が望ましい。20
%未満ではフェス中における粉末の比率が低くすぎ、ス
クリーン印刷用インクとして使用する際パターンの形態
保持性が悪く、35%以上ではポリイミド前駆体溶液の
粘度が高く攪拌が困難になる。The concentration of polyimide precursor in the polyimide precursor solution is 2
0 to 55%, and 23 to 30% is desirable. 20
If it is less than 35%, the proportion of powder in the face is too low and the shape retention of the pattern is poor when used as a screen printing ink, and if it is more than 35%, the viscosity of the polyimide precursor solution becomes high and stirring becomes difficult.
ポリイミド前駆体溶液を作るだめの反応温度としては、
40〜80℃、好ましくは40〜60℃が望ましい。4
0℃以下では重合速度が遅く、80℃以上では分子量低
下をもたらし好ましくない。The reaction temperature for making the polyimide precursor solution is:
The temperature is preferably 40-80°C, preferably 40-60°C. 4
If the temperature is below 0°C, the polymerization rate will be slow, and if it is above 80°C, the molecular weight will decrease, which is not preferable.
ポリイミド前駆体の溶液からイミド粉末を析出させるた
めのイミド閉環温度は、上限は使用する溶剤の沸点で、
下限はポリマーによって多少異なるが100〜200℃
、好ましくは110〜170℃が望5−
ましい。The upper limit of the imide ring-closing temperature for precipitating imide powder from a polyimide precursor solution is the boiling point of the solvent used;
The lower limit varies slightly depending on the polymer, but is 100 to 200°C.
, preferably 110 to 170°C.
このポリイミド粉末の懸濁液を作る工程で9次のポリイ
ミド前駆体の重合がより円滑に進むことを目的として、
チッ素フロー、真空による吸引等によりイミド閉環時発
生した縮合水を除いてもよい。・
ポリイミド粉末の懸濁液中でポリイミド前駆体を重合す
る際の重合温度としては40℃〜80℃好ましくは40
℃〜60℃が望ましい。40℃以下では重合速度が遅く
、80℃以上では分子量低下によるフェノの粘度低下を
もたらし好ましくない。In order to make the polymerization of the 9th order polyimide precursor proceed more smoothly in the process of making a suspension of this polyimide powder,
Condensed water generated during imide ring closure may be removed by nitrogen flow, vacuum suction, or the like. - The polymerization temperature when polymerizing the polyimide precursor in a suspension of polyimide powder is 40°C to 80°C, preferably 40°C.
℃~60℃ is desirable. Below 40°C, the polymerization rate is slow, and above 80°C, the viscosity of the phenol decreases due to a decrease in molecular weight, which is undesirable.
ジアミンであるH21J−R2−NH3とテトラ有機カ
ルボン酸無水物である0〈3>R′。0〉o をポリイ
ミド1\CO
粉末懸濁液中に添加する方法としては、 I(2N −
R2ポリイミド粉末/ポリイミド前駆体の重量比は70
/30〜40/60好ましくは65/35〜45155
が望ましい。H21J-R2-NH3 which is a diamine and 0<3>R' which is a tetraorganic carboxylic acid anhydride. As a method for adding 0〉o to polyimide 1\CO powder suspension, I(2N −
The weight ratio of R2 polyimide powder/polyimide precursor is 70
/30-40/60 preferably 65/35-45155
is desirable.
6一
ポリイミド粉末が7044以上では膜強度が低下し、塗
膜にひびわれ等が入りやすくなる。40%以下ではワニ
スをスクリーン印刷用インクとして使用した場合印刷パ
ターンの形態保持性が悪くなり、良好な印刷物が得られ
ない。If the 6-polyimide powder is 7044 or higher, the film strength will decrease and the coating film will be prone to cracks. If it is less than 40%, when the varnish is used as an ink for screen printing, the shape retention of the printed pattern will be poor and good printed matter will not be obtained.
さらに、一般式 ○ぐZ:ンR1ぐ3gン0とH211
1−FU2WH2から成るポリイミド粉末、ポリイミド
前駆体にはもちろん粉末形成能、膜形成能、耐熱性を著
しく損わない範囲で他のモノマーを共重合したり有機又
は/及び無機の粉末を添加してもよい。Furthermore, the general formula ○guZ:nR1gu3gn0 and H211
1-FU2WH2 polyimide powder and polyimide precursor may be copolymerized with other monomers or organic and/or inorganic powders may be added to the extent that the powder-forming ability, film-forming ability, and heat resistance are not significantly impaired. Good too.
本発明で記した製造方法により製造したポリイミドワニ
スは200℃2時向熱風オーブン中で乾燥した後の固形
分が30〜45%で東京計器(株)製BS型粘度が70
0〜2000ポイズのものである。The polyimide varnish manufactured by the manufacturing method described in the present invention has a solid content of 30 to 45% after drying in a hot air oven at 200°C for 2 hours, and a viscosity of BS type manufactured by Tokyo Keiki Co., Ltd. of 70.
It is of 0 to 2000 poise.
このワニスをカバーグラスに少量滴下し150倍の光学
顕微鏡下で粒子の分散性を調べた結果。A small amount of this varnish was dropped onto a cover glass and the dispersibility of the particles was examined under an optical microscope at 150x magnification.
粒子の二次凝集は見られなかった。又、ケンブリッジ・
インストルメント社製”’ Quantinet ”
720画像処理解析装置を用い約3〜5倍に希釈したサ
ンプルについ゛(顕微鏡倍率150倍−で′粒度分布を
a7一
定した結果粒径30 p以上の粗大粒子はなく9粒子が
均一に分散されていることがわかった。No secondary aggregation of particles was observed. Also, Cambridge
``Quantinet'' manufactured by Instrument Company
Regarding the sample diluted approximately 3 to 5 times using a 720 image processing analyzer, the particle size distribution was kept constant at a7 with a microscope magnification of 150 times. As a result, there were no coarse particles with a particle size of 30p or more, and 9 particles were uniformly dispersed. I found out that
このワニスをLT−150T にューロング精密工業(
株)製)スクリーン印刷機で′5mm X 6皿の大き
さで膜厚が50μのパターンが約200個並んだソフト
エラー防止膜用パターンをシリコンウェハー上に、シリ
コーンスキージを用い150メツシユ、エマルジョン膜
厚100μのスクリーンで印刷周期3分/枚、スキージ
ー角#69度、スクリーンとシリコンウェハーとの間隔
28■、印刷スピード4.6 an /秒、印圧1kg
/(2)2 で印刷した結果、ワニスのスクリーンから
の°゛抜け′″が良好で、パターンの一部が欠けること
もなく、連続してシリコンウェハー100枚に塗ること
ができた。さらに侍、られた塗布膜を80℃oo分+1
50℃30分+200′C30分十′550℃30分の
キュアステップでキュアしたものを。Apply this varnish to LT-150T (
Using a screen printing machine (manufactured by Co., Ltd.), a soft error prevention film pattern consisting of about 200 patterns of 50μ in the size of 5mm x 6 plates was printed onto a silicon wafer, and 150 meshes were printed using a silicone squeegee to form an emulsion film. 100μ thick screen, printing cycle 3 minutes/sheet, squeegee angle #69 degrees, distance between screen and silicon wafer 28cm, printing speed 4.6 an/sec, printing pressure 1kg
/(2) As a result of printing with 2, the varnish came out well from the screen, and 100 silicon wafers could be coated continuously without any part of the pattern being chipped.Furthermore, Samurai , the coated film was heated to 80°C for +1 min.
Cure at 50°C for 30 minutes + 200'C for 30 minutes and 550°C for 30 minutes.
150倍の顕微鏡下で観察した結果1粒子が均一に分散
した良好な塗布膜が形成されていることを確認した。As a result of observation under a microscope with a magnification of 150 times, it was confirmed that a good coating film in which single particles were uniformly dispersed was formed.
以下実施例にてさらに詳しく本発明について記8− す。The present invention will be described in further detail in Examples 8- vinegar.
実施例1
N−メチル−2−ピロリドン(以下NMPと略す)溶媒
695.6gを三ツ口21のフラスコに秤取する。これ
にジアミノジフェニルエーテル(以下DAEと略す)1
20.1gを50℃で溶媒を攪拌しながら加え、完全に
溶解する。DABが完全に溶解した後無水ピロメリット
酸(以下PMDAと略す)124.5gを溶液を攪拌し
ながら少しずつ加える。Example 1 695.6 g of N-methyl-2-pyrrolidone (hereinafter abbreviated as NMP) solvent was weighed into a three-necked 21 flask. To this, diaminodiphenyl ether (hereinafter abbreviated as DAE) 1
Add 20.1 g of the solvent at 50° C. while stirring to completely dissolve. After DAB was completely dissolved, 124.5 g of pyromellitic anhydride (hereinafter abbreviated as PMDA) was added little by little while stirring the solution.
DABとPMDAが反応し2反応熱で系内の温度が5〜
10℃上昇する。60分反応させた後80℃に系内温度
を昇温しさらに、60分反応させる。この時系内は密閉
系かN2フロー下に保つ。80℃で60分反応させた後
、冷却管をつけて密閉系で系内温度を150℃に上昇さ
せポリイミド粉末を析出させる。150℃で1.5〜2
0時間反応させポリイミド粉末を析出させ、その後70
℃に降温する。70℃に系内がなった所でDAB 94
.3gを入れその後t−<”にベンゾフェノンテトラカ
ルボン酸無水物C以下BT DAと略す)159.5g
を入れ反応させる。DAB and PMDA react and the temperature in the system increases from 5 to 5 due to the heat of 2 reactions.
The temperature increases by 10℃. After reacting for 60 minutes, the temperature inside the system was raised to 80° C., and the reaction was further continued for 60 minutes. This time frame is kept in a closed system or under N2 flow. After reacting at 80° C. for 60 minutes, the system temperature was raised to 150° C. in a closed system with a cooling pipe attached to precipitate polyimide powder. 1.5-2 at 150℃
The reaction was carried out for 0 hours to precipitate polyimide powder, and then for 70 hours.
The temperature drops to ℃. DAB 94 when the temperature inside the system reaches 70℃
.. Add 3g of benzophenonetetracarboxylic anhydride (hereinafter referred to as BTDA) to t-<” (abbreviated as BTDA) 159.5g
and react.
9−
約1時間反応させた所でBS型粘度計(東京計器(株)
製)で粘度を測定し、粘度を1000ポイズ士200ポ
イズに合わす。粘度が低い場合はBTDAを少量添加し
、高い場合はNMPで希釈する。粘度が合った所でさら
に1時間反応させ取り出す。この方、法で作成したワニ
スは粉末/バインダー−=171にもかかわらず粉末の
分散性が良好であることを顕微鏡及び画像処理解析装置
を用いて確めた。9- After reacting for about 1 hour, use a BS viscometer (Tokyo Keiki Co., Ltd.)
Measure the viscosity using a 1000 to 200 poise product. If the viscosity is low, add a small amount of BTDA, if the viscosity is high, dilute with NMP. When the viscosity matches, let it react for another hour and take it out. It was confirmed using a microscope and an image processing analysis device that the varnish prepared by this method had good powder dispersibility despite the powder/binder ratio being 171.
このワニスをスクリーン印刷機で印刷した結果。The result of printing this varnish with a screen printing machine.
ワニスのスクリーンからの「抜け」が良好で、多数回印
刷が可能であった。さらに得られた塗布膜をキュアした
結果、良好なポリイミド膜からなるパターンが得られた
。The varnish "released" well from the screen, and multiple printings were possible. Furthermore, as a result of curing the obtained coating film, a pattern consisting of a good polyimide film was obtained.
実施例2
実施例1において一1!IMP単独浴剤の代りに11M
P/エチルセロソルブ(以下EC8と略す)=8571
5 の混合溶剤系を用いて実施例1と全く同様な方法で
ワニスを作成した。Example 2 -1 in Example 1! 11M instead of IMP single bath salt
P/ethyl cellosolve (hereinafter abbreviated as EC8) = 8571
A varnish was prepared in exactly the same manner as in Example 1 using the mixed solvent system of Example 5.
できたワニスをLT−15Gスクリ一ン印刷機で印刷し
た結果、良好な印刷性を持ち、実施例1と同−のキュア
ステップでキュアした結果、良好なポリイミド膜から成
るパターンが得られた。When the resulting varnish was printed using an LT-15G screen printer, it had good printability, and when cured using the same curing step as in Example 1, a good pattern consisting of a polyimide film was obtained.
比較例1
NMP 695.6gを三ツロ21フラスコに秤取す
る。これにDAli:120.1gを5D℃で溶媒を攪
拌しながら加え、完全に溶解する。DAgが完溶したら
PMDA124.3gを少しずつ加え50℃で50分反
応させる。この後80℃に昇温してさらに50分反応さ
せる。この後150℃に昇温し、20時間150℃で反
応させポリイミド粉末を析出させる。Comparative Example 1 695.6 g of NMP was weighed into a Mitsuro 21 flask. To this, 120.1 g of DAli was added at 5D° C. while stirring the solvent, and completely dissolved. When DAg is completely dissolved, 124.3 g of PMDA is added little by little and reacted at 50°C for 50 minutes. Thereafter, the temperature was raised to 80°C and the reaction was continued for an additional 50 minutes. Thereafter, the temperature was raised to 150°C, and a reaction was carried out at 150°C for 20 hours to precipitate polyimide powder.
この粉末を3Gのガラスフィルターでろ過し、150℃
で1昼夜真空乾燥し、ポリイミド粉末を作成する。This powder was filtered through a 3G glass filter and heated to 150°C.
Vacuum drying was carried out for one day and night to create polyimide powder.
別に21の三ツロフラスコにNMP695.6gを取り
、これに70℃で指押しなからDAE94.3gを入れ
完溶させる。DAREが完溶した後攪拌下でBTDA1
59.3gを加え2時間反応させてポリアミド酸を作成
する。できだポリアミド酸溶液中に先に作成したポリイ
ミド粉末を少しずつ加えワニスを作成した。このワニス
を顕微鏡画像処理解析装置で観察すると多数の二次凝集
体が見られ、粉末が均一にバインダー中に分散していな
いことがわかったこのワニスを使ってスクリーン印刷し
た所、ワニスのスクリーンからの「抜け」が悪く、多数
回印刷ができず、得られた塗布膜も二次凝集体が散見ら
れ゛、均一な塗布膜が得られなかった。Separately, 695.6 g of NMP was placed in a Mitsuro flask (No. 21), and 94.3 g of DAE was added thereto at 70° C. until completely dissolved. After DARE is completely dissolved, add BTDA1 under stirring.
59.3g was added and reacted for 2 hours to produce polyamic acid. The polyimide powder prepared earlier was added little by little to the resulting polyamic acid solution to prepare a varnish. When this varnish was observed using a microscope image processing analyzer, a large number of secondary aggregates were observed, indicating that the powder was not uniformly dispersed in the binder.When screen printing was performed using this varnish, the varnish screen "Shedding" was poor, making it impossible to print multiple times, and secondary aggregates were observed here and there in the coating film obtained, making it impossible to obtain a uniform coating film.
特許出願人 東 し 株 式 会 社12−Patent Applicant Higashi Shikaisha Co., Ltd. 12-
Claims (1)
させ、仰られたポリイミド前1駆体浴液をイミド閉環高
度で加熱してポリイミド粉末を析出させ、得られたポリ
イミド粉末の懸濁液中で、テトラ有機カルボン酸無水物
とジアミンを反応させポリイミド前駆体を形成すること
を特徴とするポリイミドワニスの製造方法。A tetraorganic carboxylic acid anhydride and a diamine are reacted in a solvent, and the polyimide precursor bath solution is heated at an imide ring-closing degree to precipitate polyimide powder, and in a suspension of the obtained polyimide powder. A method for producing a polyimide varnish, which comprises reacting a tetraorganic carboxylic acid anhydride and a diamine to form a polyimide precursor.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7133382A JPS58189260A (en) | 1982-04-30 | 1982-04-30 | Production of polyimide varnish |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP7133382A JPS58189260A (en) | 1982-04-30 | 1982-04-30 | Production of polyimide varnish |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS58189260A true JPS58189260A (en) | 1983-11-04 |
JPH021192B2 JPH021192B2 (en) | 1990-01-10 |
Family
ID=13457494
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP7133382A Granted JPS58189260A (en) | 1982-04-30 | 1982-04-30 | Production of polyimide varnish |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS58189260A (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011173423A (en) * | 2005-04-04 | 2011-09-08 | Ube Industries Ltd | Copper-clad laminated substrate |
-
1982
- 1982-04-30 JP JP7133382A patent/JPS58189260A/en active Granted
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP2011173423A (en) * | 2005-04-04 | 2011-09-08 | Ube Industries Ltd | Copper-clad laminated substrate |
Also Published As
Publication number | Publication date |
---|---|
JPH021192B2 (en) | 1990-01-10 |
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