JPS6341873B2 - - Google Patents
Info
- Publication number
- JPS6341873B2 JPS6341873B2 JP55083537A JP8353780A JPS6341873B2 JP S6341873 B2 JPS6341873 B2 JP S6341873B2 JP 55083537 A JP55083537 A JP 55083537A JP 8353780 A JP8353780 A JP 8353780A JP S6341873 B2 JPS6341873 B2 JP S6341873B2
- Authority
- JP
- Japan
- Prior art keywords
- frit
- organic vehicle
- temperature
- vitreous frit
- organic
- 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.)
- Expired
Links
- 238000000034 method Methods 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 16
- 230000008018 melting Effects 0.000 claims description 16
- 239000010953 base metal Substances 0.000 claims description 15
- 239000000758 substrate Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 9
- 229910052709 silver Inorganic materials 0.000 description 8
- 239000004332 silver Substances 0.000 description 8
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 229920000620 organic polymer Polymers 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910052802 copper Inorganic materials 0.000 description 4
- 239000010949 copper Substances 0.000 description 4
- 229910052759 nickel Inorganic materials 0.000 description 4
- 238000011946 reduction process Methods 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004020 conductor Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 229910000679 solder Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000010946 fine silver Substances 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
Description
【発明の詳細な説明】
本発明は、セラミツク基板等の素体上に卑金属
より成る導電性皮膜を形成する方法に関する。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for forming a conductive film made of a base metal on an element body such as a ceramic substrate.
磁器コンデンサの電極やIC基板の導体パター
ン等を形成する場合、従来は、素体にフリツト含
有銀ペーストを塗布し、かつ焼付けて電極とする
のが一般的であつた。しかし、銀焼付電極である
と、半田付時に電極銀が半田中に拡散移行する。
いわゆる半田喰われ現象による容量不足、電極密
着強度の低下や、シルバーマイグレーシヨンによ
る絶縁劣化等の問題を生じ易く、また資源的に乏
しく高価な銀を多量に使用しなければならないた
め、コスト高になるという欠点がある。こうした
銀焼付電極の欠点を除去するため、最近、ニツケ
ル、銅等の卑金属を用いた電極の形成方法が提案
されている。この卑金属を用いた電極形成方法
は、第１図に示すように、ニツケル微粉末または
銅微粉末と、ガラス質フリツトと、解重合性有機
高分子物質より成る有機質のベヒクルとを適当な
割合で混合して卑金属ペーストを調製し、これを
スクリーン印刷法などの手段によつてセラミツク
基板等の基体上に所定パターンとなるように印刷
塗布し、次に乾燥させた後、真空中または不活性
雰囲気中で前記有機質のベヒクルをバーンアウト
し、更にこの後、真空中または不活性雰囲気中で
焼付けていた。 When forming electrodes for ceramic capacitors, conductor patterns for IC boards, etc., it has conventionally been common to apply a frit-containing silver paste to an element body and then bake it to form the electrode. However, if the electrode is baked with silver, the electrode silver will diffuse into the solder during soldering.
Problems such as a lack of capacity due to the so-called solder eating phenomenon, a decrease in electrode adhesion strength, and insulation deterioration due to silver migration are likely to occur, and the cost is high because a large amount of silver, which is scarce and expensive, must be used. It has the disadvantage of becoming. In order to eliminate these drawbacks of baked silver electrodes, methods for forming electrodes using base metals such as nickel and copper have recently been proposed. As shown in Figure 1, this method of forming electrodes using base metals involves mixing fine nickel powder or fine copper powder, glassy frit, and an organic vehicle made of a depolymerizable organic polymer material in appropriate proportions. A base metal paste is prepared by mixing, and this is printed and coated onto a substrate such as a ceramic substrate in a predetermined pattern by means such as screen printing, and then dried and then placed in a vacuum or in an inert atmosphere. The organic vehicle was burnt out in a vacuum and then baked in a vacuum or an inert atmosphere.
銀微粉末を主成分とする銀ペーストであれば、
空気中等の酸化性雰囲気中で焼付けて導電性皮膜
を形成することができるが、ニツケル、銅等の卑
金属の場合は、空気中で加熱したのでは卑金属が
金属酸化物となり、電極または導体としての機能
を果さなくなるため、真空中または不活性雰囲気
中で有機質のベヒクルをバーンアウトし、焼付け
なければならない。したがつて、有機質のベヒク
ルとしては、実質的に酸素の存在しない雰囲気で
加熱処理した場合でも完全に分解除去し得、しか
も減圧状態でも分解して単量体などの低分子化合
物になる物質、すなわち解重合性有機高分子物質
を使用しなければならない。このためベヒクルの
選択幅が非常に狭くなるという点があつた。 If it is a silver paste whose main component is fine silver powder,
A conductive film can be formed by baking in an oxidizing atmosphere such as air, but in the case of base metals such as nickel and copper, heating in air turns the base metal into a metal oxide, making it difficult to use as an electrode or conductor. The organic vehicle must be burnt out and baked in a vacuum or in an inert atmosphere to prevent it from functioning. Therefore, organic vehicles include substances that can be completely decomposed and removed even when heated in an atmosphere substantially free of oxygen, and that decompose even under reduced pressure to form low-molecular compounds such as monomers. That is, a depolymerizable organic polymer substance must be used. For this reason, the range of vehicle selection was extremely narrow.
また、有機質ベヒクルとして解重合性有機高分
子物質を使用し、真空中または不活性雰囲気中で
バーンアウトした場合、ベヒクルを完全にバーン
アウトすることができず、どうしてもベヒクルが
残つてしまう。このため、バーンアウト工程後、
第２図に示すように、卑金属ペースト２を被着さ
せた多数個の電子部品１を重ねた状態で焼付ける
と、残存している有機質ベヒクルによつて電子部
品１の各々が互に結着してしまうという問題があ
り、この欠点を避けるために、電子部品１の各々
を個別的に焼付けしなければならず、焼付け処理
の生産性が悪いという欠点もあつた。 Furthermore, when a depolymerizable organic polymer substance is used as the organic vehicle and burnout is performed in a vacuum or an inert atmosphere, the vehicle cannot be completely burnt out and the vehicle inevitably remains. Therefore, after the burnout process,
As shown in FIG. 2, when a large number of electronic components 1 coated with base metal paste 2 are baked in a stacked state, each of the electronic components 1 is bonded to each other by the remaining organic vehicle. In order to avoid this problem, each of the electronic components 1 must be individually baked, which also has the disadvantage of poor productivity in the baking process.
本発明は上述する欠点を除去し、有機質ベヒク
ルの選択幅が非常に広く、しかも有機質ベヒクル
を完全にバーンアウトし、焼付処理量を飛躍的に
向上させ得るようにした導電性皮膜の形成方法を
提供することを目的とする。 The present invention eliminates the above-mentioned drawbacks, provides a method for forming a conductive film that has a very wide range of organic vehicles to choose from, and that can completely burn out the organic vehicle and dramatically improve the baking throughput. The purpose is to provide.
上記目的を達成するため、本発明に係る導電性
皮膜の形成方法は、基体上に、卑金属微粉末を導
電成分としガラス質フリツト及び有機質ビヒクル
を含有する導電性ペーストを塗布し、これを前記
ガラス質フリツトの溶解温度よりも低い温度で空
気中で加熱して前記導電性ペーストに含まれる有
機質ベヒクルをバーンアウトした後、前記ガラス
質フリツトの溶解温度よりも低い温度で還元性雰
囲気中で加熱して還元し、次に不活性雰囲気中に
おいて前記ガラス質フリツトの溶解温度付近で加
熱して焼付けることを特徴とする。 In order to achieve the above object, the method for forming a conductive film according to the present invention involves applying a conductive paste containing a base metal fine powder as a conductive component, a glassy frit, and an organic vehicle onto a substrate; The conductive paste is heated in air at a temperature lower than the melting temperature of the vitreous frit to burn out the organic vehicle contained in the conductive paste, and then heated in a reducing atmosphere at a temperature lower than the melting temperature of the vitreous frit. The vitreous frit is then reduced by heating in an inert atmosphere at a temperature close to the melting temperature of the vitreous frit.
第３図は本発明に係る導電性皮膜の形成方法を
説明する図である。 FIG. 3 is a diagram illustrating a method for forming a conductive film according to the present invention.
まず、ニツケル微粉末または銅微粉末と、ガラ
ス質フリツトと有機質ベヒクルとを、たとえば
65：1.5：33.5の割合で混合して卑金属を主成分
とする導電性ペーストを調製し、これをスクリー
ン印刷等の手段によつてセラミツク基板等の基板
上の所定パターンとなるように塗布する。この場
合、従来は有機質ベヒクルとして解重合性有機高
分子物質を用いることが必須であつたが、本発明
においてはこのような制限はない。銀ペースト等
で用いられている有機質バインダ、たとえばレジ
ン、ソルベント等を使用することができる。 First, fine nickel powder or fine copper powder, a glassy frit, and an organic vehicle are mixed together, for example.
A conductive paste containing base metal as a main component is prepared by mixing in a ratio of 65:1.5:33.5, and this is applied to a substrate such as a ceramic substrate in a predetermined pattern by means such as screen printing. In this case, conventionally it has been essential to use a depolymerizable organic polymer substance as the organic vehicle, but the present invention is not subject to such limitations. Organic binders used in silver paste and the like, such as resins and solvents, can be used.
次に、導電性ペーストを乾燥させた後、空気中
で有機質ベヒクルをバーンアウトする。焼成温度
は300〜400℃程度が適当である。この温度範囲は
導電性ペーストに含まれるガラス質フリツトの溶
解温度600〜950℃よりも低い範囲であり、有機質
ビヒクルのバーンアウト工程においてガラス質フ
リツトが溶解することがない。このため、ガラス
質フリツト溶解によつて有機質ビヒクルのバーン
アウトが妨げられることがなく、確実にバーンア
ウトできる。このように、空気中でバーンアウト
する構成であるから、有機質ベヒクルとして従来
の解重合性高分子物質を使用する必要がなくな
り、有機質ベヒクルの選択幅が著るしく拡張され
る。また、レジン、ソルベント等の有機添加物
は、完全に分解遊離され、残存することがない。
さらに、雰囲気形成のための特別の設備を必要と
せず、設備費が安価になる。 Next, after drying the conductive paste, the organic vehicle is burnt out in air. The appropriate firing temperature is about 300 to 400°C. This temperature range is lower than the melting temperature of 600 to 950° C. of the vitreous frit contained in the conductive paste, and the vitreous frit does not melt during the burnout process of the organic vehicle. Therefore, burnout of the organic vehicle is not hindered by the melting of the vitreous frit, and burnout can be ensured. As described above, since it is configured to burn out in air, there is no need to use a conventional depolymerizable polymer substance as an organic vehicle, and the range of selection of organic vehicles is significantly expanded. Furthermore, organic additives such as resins and solvents are completely decomposed and released, and do not remain.
Furthermore, no special equipment is required for creating an atmosphere, resulting in lower equipment costs.
次に、この基体を水素雰囲気中において、酸化
された皮膜を還元する。これにより、前工程のバ
ーンアウトにより酸化されたニツケル粒子もしく
は銅粒子が還元され、卑金属の導電性皮膜が形成
される。処理温度は300〜400℃程度が適当であ
る。この温度範囲は導電性ペーストに含まれるガ
ラス質フリツトの溶解温度600〜950℃よりも低い
範囲であり、還元工程においてガラス質フリツト
が溶解することがない。このため、ガラス質フリ
ツト溶解によつて酸化皮膜の還元が妨げられるこ
とがなく、酸化皮膜をその全厚みに亙つて略均一
に還元し、導電度の高い卑金属導電性皮膜の形成
できる。 Next, this substrate is placed in a hydrogen atmosphere to reduce the oxidized film. As a result, the nickel particles or copper particles oxidized by burnout in the previous process are reduced, and a base metal conductive film is formed. Appropriate treatment temperature is about 300 to 400°C. This temperature range is lower than the melting temperature of 600 to 950°C of the vitreous frit contained in the conductive paste, and the vitreous frit does not melt in the reduction process. Therefore, the reduction of the oxide film is not hindered by the glassy frit melting, and the oxide film can be reduced substantially uniformly over its entire thickness, making it possible to form a base metal conductive film with high electrical conductivity.
次に、この還元工程の終了後、たとえば窒素ガ
ス等の不活性雰囲気中で焼付けを行なう。焼付温
度は600〜950℃程度が適当である。この温度範囲
は卑金属導電性皮膜に含まれるガラス質フリツト
の溶解温度領域であり、ガラス質フリツトを確実
に溶解させることができる。前工程において金属
化されたニツケル粒子もしくは銅粒子は、溶解し
たフリツトにより、基体上に強固に焼結される。
この場合、バーンアウト工程において、有機質ベ
ヒクルが完全に遊離分解されているので、導電性
皮膜を形成した基体を多数個バラ積みした状態で
焼付けても、基体が互に結着することがない。し
たがつて、焼付処理量を従来より大幅に増大させ
ることが可能となる。 Next, after this reduction step is completed, baking is performed in an inert atmosphere such as nitrogen gas. Appropriate baking temperature is about 600 to 950°C. This temperature range is the melting temperature range of the vitreous frit contained in the base metal conductive film, and the vitreous frit can be reliably melted. The nickel or copper particles metallized in the previous step are firmly sintered onto the substrate by the molten frit.
In this case, in the burnout step, the organic vehicle is completely decomposed to liberate, so even if a large number of substrates on which conductive films are formed are stacked and baked, the substrates will not stick to each other. Therefore, it becomes possible to significantly increase the amount of printing processing compared to the conventional method.
第４図は上述したバーンアウト工程、還元工程
および焼付工程の焼成プログラムの一例を示し、
横軸に時間（分）を、縦軸に温度（℃）をとつて
ある。イはバーンアウト工程、ロは還元工程、ハ
は焼付工程である。バーンアウト工程イでは、一
定の傾斜で約350℃まで昇温させた後、約20分間
の定温期間を設けた。また還元工程ロでは、炉内
をH2／N2＝１／99.9〜100／０の還元性雰囲気と
し、350℃の定温度で還元処理した。さらに焼付
工程ハでは、H2／N2の還元性雰囲気を窒素N2に
よる不活性雰囲気に変えた後、600℃〜950℃まで
昇温させ、この温度に保つたまま、約20分間焼付
け処理を行なつた。 FIG. 4 shows an example of a firing program for the burnout process, reduction process, and baking process described above.
The horizontal axis shows time (minutes), and the vertical axis shows temperature (°C). A is a burnout process, B is a reduction process, and C is a baking process. In the burnout step 1, the temperature was raised to about 350°C at a constant slope, and then a constant temperature period of about 20 minutes was provided. In the reduction step B, the inside of the furnace was made into a reducing atmosphere of H 2 /N 2 = 1/99.9 to 100/0, and reduction treatment was performed at a constant temperature of 350°C. Furthermore, in the baking process C, after changing the reducing atmosphere of H 2 /N 2 to an inert atmosphere of nitrogen N 2 , the temperature is raised to 600°C to 950°C, and baking is performed for about 20 minutes while maintaining this temperature. I did this.
以上述べたように本発明に係る導電性皮膜の形
成方法によれば、次のような効果が得られる。 As described above, according to the method for forming a conductive film according to the present invention, the following effects can be obtained.
(a) 空気中で加熱して導電性ペーストに含まれる
有機質ベヒクルをバーンアウトするから、有機
質ビヒクルを解重合性有機高分子物質とする必
要がなく、任意の有機質とすることができ、そ
の選択幅を著しく拡張すると共に、バラ積みに
よる焼付けを可能にし、焼付処理を飛躍的に向
上させることができる。(a) Since the organic vehicle contained in the conductive paste is burnt out by heating in the air, the organic vehicle does not need to be a depolymerizable organic polymer material, and can be any organic material, which can be selected. In addition to significantly expanding the width, it is possible to bake in bulk, and the baking process can be dramatically improved.
(b) 有機質ビヒクルをバーンアウトする場合、導
電性ペーストに含まれるガラス質フリツトの溶
解温度よりも低い温度で加熱するので、有機質
ビヒクルのバーンアウト工程においてガラス質
フリツトが溶解することがない。このため、ガ
ラス質フリツト溶解によつて有機質ビヒクルの
バーンアウトが妨げられることがなく、確実に
バーンアウトできる。(b) When burning out the organic vehicle, heating is performed at a temperature lower than the melting temperature of the vitreous frit contained in the conductive paste, so the vitreous frit does not melt during the burnout process of the organic vehicle. Therefore, burnout of the organic vehicle is not hindered by the melting of the vitreous frit, and burnout can be ensured.
(c) バーンアウト工程の後に、ガラス質フリツト
の溶解温度よりも低い温度で還元性雰囲気中で
加熱して還元するので、還元工程においてガラ
ス質フリツトが溶解することがない。このた
め、ガラス質フリツト溶解によつて酸化皮膜の
還元が妨げられることがなく、酸化皮膜をその
全厚みに亙つて略均一に還元し、導電度の高い
卑金属導電性皮膜を形成できる。(c) After the burnout process, the vitreous frit does not melt in the reduction process because it is heated in a reducing atmosphere at a temperature lower than the melting temperature of the vitreous frit. Therefore, the reduction of the oxide film is not hindered by the glassy frit melting, and the oxide film can be reduced substantially uniformly over its entire thickness to form a highly conductive base metal conductive film.
(d) 還元工程の後、不活性雰囲気中においてガラ
ス質フリツトの溶解温度付近で加熱して焼付け
るので、再酸化を防止しつつ、ガラス質フリツ
トを確実に溶解させて基体上に密着させ、導電
度が高く、密着強度の高い卑金属導電性皮膜を
形成できる。(d) After the reduction step, the vitreous frit is heated and baked in an inert atmosphere near the melting temperature of the vitreous frit, so that the vitreous frit is reliably melted and adhered to the substrate while preventing re-oxidation. A base metal conductive film with high conductivity and adhesive strength can be formed.
第１図は従来の導電性皮膜の形成方法を説明す
る図、第２図はその欠点を説明する図、第３図は
本発明に係る導電性皮膜の形成方法を説明する
図、第４図はその焼成プログラムの一例を示す図
である。
FIG. 1 is a diagram explaining the conventional method of forming a conductive film, FIG. 2 is a diagram explaining its drawbacks, FIG. 3 is a diagram explaining the method of forming a conductive film according to the present invention, and FIG. is a diagram showing an example of the firing program.
Claims (1)
質フリツト及び有機質ビヒクルを含有する導電性
ペーストを塗布し、これを前記ガラス質フリツト
の溶解温度よりも低い温度で空気中で加熱して前
記導電性ペーストに含まれる有機質ベヒクルをバ
ーンアウトした後、前記ガラス質フリツトの溶解
温度よりも低い温度で還元性雰囲気中で加熱して
還元し、次に不活性雰囲気中において前記ガラス
質フリツトの溶解温度付近で加熱して焼付けるこ
とを特徴とする導電性皮膜の形成方法。1. A conductive paste containing a base metal fine powder as a conductive component, a vitreous frit, and an organic vehicle is applied onto a substrate, and this is heated in air at a temperature lower than the melting temperature of the vitreous frit to form the conductive paste. After burning out the organic vehicle contained in the paste, it is reduced by heating in a reducing atmosphere at a temperature lower than the melting temperature of the vitreous frit, and then heated in an inert atmosphere near the melting temperature of the vitreous frit. A method for forming a conductive film, characterized by heating and baking with.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8353780A JPS5711881A (en) | 1980-06-20 | 1980-06-20 | Formation of electroconductive film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8353780A JPS5711881A (en) | 1980-06-20 | 1980-06-20 | Formation of electroconductive film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5711881A JPS5711881A (en) | 1982-01-21 |
| JPS6341873B2 true JPS6341873B2 (en) | 1988-08-19 |
Family
ID=13805243
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8353780A Granted JPS5711881A (en) | 1980-06-20 | 1980-06-20 | Formation of electroconductive film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS5711881A (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63233090A (en) * | 1987-03-23 | 1988-09-28 | 日本電産コパル株式会社 | Manufacture of copper circuit low temperature burnt substrate |
-
1980
- 1980-06-20 JP JP8353780A patent/JPS5711881A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5711881A (en) | 1982-01-21 |
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