JPH05128910A - Conductor paste - Google Patents
Conductor pasteInfo
- Publication number
- JPH05128910A JPH05128910A JP31857391A JP31857391A JPH05128910A JP H05128910 A JPH05128910 A JP H05128910A JP 31857391 A JP31857391 A JP 31857391A JP 31857391 A JP31857391 A JP 31857391A JP H05128910 A JPH05128910 A JP H05128910A
- Authority
- JP
- Japan
- Prior art keywords
- paste
- conductor paste
- teo
- weight
- palladium
- 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
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Parts Printed On Printed Circuit Boards (AREA)
- Paints Or Removers (AREA)
- Conductive Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は特にＲｕＯ2 系抵抗体の
電極として好適な導体ペーストに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a conductor paste suitable as an electrode for RuO 2 type resistors.
【０００２】[0002]
【従来の技術】厚膜抵抗体の電極材料として、通常銀と
パラジウムを含む複合粉末と、ガラス粉末およびＢｉ2
Ｏ3 を含有するＡｇ／Ｐｄ系導体ペーストが用いられて
いる。2. Description of the Related Art As an electrode material of a thick film resistor, a composite powder usually containing silver and palladium, a glass powder and Bi 2 are used.
An Ag / Pd-based conductor paste containing O 3 is used.
【０００３】銀とパラジウムを含む複合粉末としては、
銀とパラジウムの混合粉の外、銀パラジウム合金粉、銀
パラジウム共沈粉またはこれらと銀粉及び／又はパラジ
ウム粉との混合粉が用いられ、通常Ａｇ／Ｐｄ比が１．
５〜１９になる組成でペースト固形分中に８５〜９５重
量％含有される。As a composite powder containing silver and palladium,
In addition to a mixed powder of silver and palladium, a silver-palladium alloy powder, a silver-palladium co-precipitated powder, or a mixed powder of these and a silver powder and / or a palladium powder is used, and the Ag / Pd ratio is usually 1.
It has a composition of 5 to 19 and is contained in the paste solid content in an amount of 85 to 95% by weight.
【０００４】ガラス粉末は、ＰｂＯ−Ｂ2 Ｏ3 −ＳｉＯ
2 系ガラス、ＰｂＯ−Ｂ2 Ｏ3 −ＺｎＯ系ガラス等が使
用される場合が多い。導体ペーストは、セラミック基板
に印刷、焼成されるため、ガラスはセラミック基板の熱
膨張係数に近い値の熱膨張係数を持つものが使われてお
り、例えば、アルミナ基板に対しては、７０〜７５×１
０-6／℃程度の熱膨張係数をもつガラスが用いられる。
ガラス粉末はペースト固形分中に２〜７重量％含有され
る。又、酸化ビスマス粉末は、ペースト固形分中に３〜
１３重量％含有される。The glass powder is PbO-B 2 O 3 -SiO.
2 based glass, often PbO-B 2 O 3 -ZnO based glass or the like is used. Since the conductor paste is printed and fired on a ceramic substrate, glass having a coefficient of thermal expansion close to that of the ceramic substrate is used. For example, 70 to 75 for an alumina substrate. × 1
Glass having a coefficient of thermal expansion of about 0 -6 / ° C is used.
The glass powder is contained in the paste solid content in an amount of 2 to 7% by weight. Further, the bismuth oxide powder has a solid content of 3 to 3%.
13% by weight is contained.
【０００５】これらの固形物粉末を均一に混合してセラ
ミック基板上に印刷できるようにするために、固形分を
ビヒクルと混練してペースト状の組成物にする。このビ
ヒクルとして有機溶剤と樹脂の混合物が用いられてい
る。有機溶剤としてはターピネオール、ブチルカルビト
ール等が、又、樹脂としてはエチルセロルース、ニトロ
セルロース、ポリ酢酸ビニル等が用いられる。ターピネ
オール中にエチルセルロースを約２０重量％含有するも
のが用いられることが多い。また、印刷を円滑にするた
め、銀とパラジウムを含む複合粉末、ガラス粉末及び酸
化ビスマス粉末は３２５メッシュより小さいものが用い
られる場合が多い。In order to uniformly mix these solid powders so that they can be printed on a ceramic substrate, the solids are kneaded with a vehicle to form a paste-like composition. A mixture of an organic solvent and a resin is used as this vehicle. As the organic solvent, terpineol, butyl carbitol, etc. are used, and as the resin, ethyl cellulose, nitrocellulose, polyvinyl acetate, etc. are used. Terpineol containing about 20% by weight of ethyl cellulose is often used. Further, in order to facilitate printing, the composite powder containing silver and palladium, the glass powder, and the bismuth oxide powder are often smaller than 325 mesh.
【０００６】[0006]
【発明が解決しようとする課題】厚膜抵抗器を製造する
場合、導体ペーストの印刷、焼成により、セラミック基
板上に電極を形成した後、電極間に抵抗体ペーストを印
刷、焼成して抵抗体を形成するが、抵抗体がＲｕＯ2 を
導電成分として含有すると、この抵抗体ペーストを焼成
した際に電極の露出部が黒く変色することがある。この
変色（「ステイン」と称する）は、ＲｕＯ2 含有率の高
い抵抗体ペーストを印刷した基板を多数、密集して焼成
するときに顕著に発生することから、抵抗体ペースト焼
成時に抵抗体から気体状の酸化ルテニウム（ＲｕＯ3 、
ＲｕＯ4 等）が揮発し、これが電極中のＢｉ2 Ｏ3 と反
応してＢｉ2 Ｒｕ2 Ｏ7 を生成するのが原因であろうと
考えられている。When manufacturing a thick film resistor, a conductor paste is printed and fired to form electrodes on a ceramic substrate, and then a resistor paste is printed and fired between the electrodes to form a resistor. However, if the resistor contains RuO 2 as a conductive component, the exposed portion of the electrode may turn black when the resistor paste is fired. This discoloration (referred to as “stain”) occurs remarkably when a large number of substrates on which a resistor paste having a high RuO 2 content is printed are densely fired. Ruthenium oxide (RuO 3 ,
It is believed that this is due to the volatilization of RuO 4 etc.), which reacts with Bi 2 O 3 in the electrode to produce Bi 2 Ru 2 O 7 .
【０００７】電極にステインがあると半田濡れ性が低下
し、リード線の半田付けが困難になる。このようなステ
インの発生を防止するには導体ペースト中のＢｉ2 Ｏ3
を少なくすれば良いが、そのようにすると電極と基板と
の接着強度が低下するだけでなく、半田濡れ性、半田耐
食性も低下するので、むやみにＢｉ2 Ｏ3 含有率を低下
させるわけにはいかない。このためＢｉ2 Ｏ3 含有率を
幾分低くした導体ペーストを用い、抵抗体の焼成に際し
ては基板の間隔を空けるようにしている。しかしながら
このような焼成の仕方は能率的でない。If the electrodes have stains, the solder wettability deteriorates, and it becomes difficult to solder the lead wires. In order to prevent the occurrence of such stain, Bi 2 O 3 in the conductor paste is
However, if so, not only the adhesive strength between the electrode and the substrate is lowered, but also the solder wettability and the solder corrosion resistance are lowered. Therefore, it is not possible to unnecessarily reduce the Bi 2 O 3 content. It doesn't. For this reason, a conductor paste having a slightly lower Bi 2 O 3 content is used, and a space is provided between the substrates when firing the resistor. However, such a firing method is not efficient.
【０００８】この問題を解決するために、酸化ビスマス
の代わりにＢｉ2 Ｏ3 とＶ2 Ｏ5 の溶融粉砕物を用いる
という手段（特公平３−１１４８５）が提案されてい
る。しかしながらＶ2 Ｏ5 は生体中のいろいろな代謝作
用に影響を与えることが認められており、脂質、とりわ
け燐脂質・コレステロールの代謝、アミノ酸その他の酸
化酵素、鉄の代謝、アドレナリンの分泌を阻害するとい
われている。このため、Ｖ2 Ｏ5 を用いなくともステイ
ンが発生しにくい導体ペーストの開発が強く要請されて
いた。In order to solve this problem, a means of using a melt pulverized product of Bi 2 O 3 and V 2 O 5 instead of bismuth oxide (Japanese Patent Publication No. 3-11485) has been proposed. However, V 2 O 5 is known to affect various metabolic actions in the living body, and it inhibits the metabolism of lipids, especially phospholipids / cholesterol, amino acids and other oxidases, iron metabolism, and adrenaline secretion. It is said. Therefore, there has been a strong demand for the development of a conductive paste that does not easily generate stains without using V 2 O 5 .
【０００９】本発明は上記事情に鑑みて為されたもので
あり、ステインが発生しにくく、半田付けが容易でしか
も基板の接着力の充分な電極が形成でき、しかも製造時
の作業環境上の問題のない導体ペーストを提供すること
を目的とする。The present invention has been made in view of the above circumstances, and it is possible to form an electrode that is less likely to cause stains, is easy to solder, and has a sufficient adhesive force to a substrate, and also to improve the working environment during manufacturing. The purpose is to provide a conductor paste that does not have any problems.
【００１０】[0010]
【課題を解決するための手段】この目的を達成するため
本発明者等が種々研究した結果、酸化ビスマスの代わり
にＢｉ2 Ｏ3 とＴｅＯ2 の溶融粉砕物を用いれば良いこ
とを見いだして本発明に到達した。さらに詳しくは、本
発明は銀とパラジウムを含む複合粉末、ガラス粉末及び
ＴｅＯ2 含有率が１５〜３２モル％であるＢｉ2 Ｏ3 −
ＴｅＯ2 溶融粉砕物を含有し、該溶融粉砕物はペースト
固形分中に２〜１１重量％含有されている点に特徴があ
る。As a result of various researches conducted by the present inventors in order to achieve this object, it was found that a fused pulverized product of Bi 2 O 3 and TeO 2 should be used instead of bismuth oxide. The invention has been reached. More specifically, the present invention provides a composite powder containing silver and palladium, a glass powder, and a Bi 2 O 3 — having a TeO 2 content of 15 to 32 mol%.
It is characterized in that it contains a TeO 2 melt pulverized product, and the melt pulverized product is contained in a paste solid content of 2 to 11 wt%.
【００１１】[0011]
【作用】Ｂｉ2 Ｏ3 −ＴｅＯ2 溶融粉砕物中のＴｅＯ2
含有率は１５〜３２モル％とする必要がある。１５モル
％未満ではステイン防止の効果が小さく、また、３２モ
ル％を超えるとステイン防止の効果が減少するとともに
半田濡れ性も低下し、電極材料として実用的でないから
である。好ましいＴｅＯ2 含有率は２０〜２８モル％で
ある。[Action] Bi 2 O 3 -TeO 2 TeO 2 of molten grind
The content must be 15 to 32 mol%. This is because if it is less than 15 mol%, the stain preventing effect is small, and if it exceeds 32 mol%, the stain preventing effect is reduced and the solder wettability is also deteriorated, which is not practical as an electrode material. A preferable TeO 2 content is 20 to 28 mol%.
【００１２】Ｂｉ2 Ｏ3 −ＴｅＯ2 溶融粉砕物は、ペー
スト固形分中に２〜１１重量％含有せしめるとよい。２
重量％未満では基板に対する接着力が充分でない。ま
た、１１重量％を超えると半田濡れ性を低下させるの
で、実用的でない。The Bi 2 O 3 -TeO 2 melt pulverized product may be contained in the paste solid content in an amount of 2 to 11% by weight. Two
If it is less than wt%, the adhesive force to the substrate is insufficient. Further, if it exceeds 11% by weight, the solder wettability is deteriorated, which is not practical.
【００１３】Ｂｉ2 Ｏ3 −ＴｅＯ2 溶融粉砕物は、Ｂｉ
2 Ｏ3 −ＴｅＯ2 を所望の割合で混合したものを１００
０℃程度にて溶融、その後急冷し、固化後粉砕して得る
ことができる。粉砕の程度は３２５メッシュより小さい
ことが望ましい。Bi 2 O 3 -TeO 2 melt pulverized product is
A mixture of 2 O 3 -TeO 2 in a desired ratio is 100
It can be obtained by melting at about 0 ° C., then rapidly cooling, solidifying and then pulverizing. It is desirable that the degree of pulverization is smaller than 325 mesh.
【００１４】本発明の導体ペーストにより形成した電極
はステインが発生しにくく、基板との接着力が充分で半
田に対する特性も良好であり、ＲｕＯ2 系抵抗体の電極
として極めて優れたものである。The electrode formed of the conductor paste of the present invention is less likely to cause stains, has sufficient adhesive strength to the substrate, and has good characteristics for soldering, and is an extremely excellent electrode for a RuO 2 type resistor.
【００１５】[0015]
【実施例】ＴｅＯ2 を１０、１５、２０、２８、３２及
び３５モル％含有するＢｉ2 Ｏ3 −ＴｅＯ2 溶融粉砕物
を用意し、該粉砕物を種々の割合で含有するＡｇ−Ｐｄ
系導体ペーストを試作し、試験に供した。各ペーストの
組成を表１に示す。表１においてＡｇは平均粒径１μｍ
の銀粉、Ｐｄは平均粒径０．２μｍのパラジウム粉、ガ
ラスは重量比でＰｂＯ：Ｂ2 Ｏ3 ：ＳｉＯ2 ＝６０：１
０：３０からなる組成のガラス粉、ビヒクルはターピネ
オール中にエチルセルロースを２０重量％含有するもの
を用いた。EXAMPLE A Bi 2 O 3 -TeO 2 melt pulverized product containing 10, 15, 20, 28, 32 and 35 mol% of TeO 2 was prepared, and Ag-Pd containing the pulverized product in various ratios was prepared.
A system conductor paste was made as a prototype and used for the test. The composition of each paste is shown in Table 1. In Table 1, Ag is an average particle size of 1 μm
Silver powder, Pd is palladium powder having an average particle size of 0.2 μm, and glass is PbO: B 2 O 3 : SiO 2 = 60: 1 by weight ratio.
As the glass powder and vehicle having a composition of 0:30, terpineol containing 20% by weight of ethyl cellulose was used.
【００１６】試験は下記の方法により行なった。 （１）ステイン ＲｕＯ2 系抵抗体の焼成の際に電極にステインが現われ
るか否かを次の方法で評価した。まず、上記導体ペース
トを２．５４ｃｍ角のアルミナ基板１枚に、１００Ω／
□級のＲｕＯ2 系抵抗体ペーストを１．８０ｃｍ角のパ
ータンで８枚印刷する。これらの基板を、導体ペースト
を同様に印刷、焼成した１枚の基板を中心に３行３列に
密接して並べてベルト式焼成炉中で焼成した１枚の基板
を中心に３行３列に密接して並べてベルト式焼成炉中で
焼成した。焼成後導体部分を観察し、変色の有無を調べ
た。変色が確認できないものを○、変色がわずかに確認
できるものを△、明らかに変色が認められるものを×と
する。The test was conducted by the following method. (1) Stain It was evaluated by the following method whether or not stain appears on the electrode during firing of the RuO 2 -based resistor. First, the above conductor paste is applied to one 2.54 cm square alumina substrate at 100 Ω /
8 sheets of □ grade RuO 2 series resistor paste are printed with a 1.80 cm square pattern. These substrates were printed in the same manner as the conductor paste, and were arranged in close contact in 3 rows and 3 columns centering on one board that was fired. They were closely arranged and fired in a belt-type firing furnace. After firing, the conductor portion was observed and examined for discoloration. The case where no discoloration can be confirmed is indicated by O, the case where slight discoloration can be confirmed is indicated by Δ, and the case where obvious discoloration is observed is indicated by X.
【００１７】（２）接着強度 ２．５４ｃｍ角のアルミナ基板に導体ペーストを２ｍｍ
角パータンを５個印刷し、８５０℃で焼成後、導体部に
０．６５ｍｍφの錫めっき銅線を鉛３７重量％、残部錫
のＰｂ−Ｓｎ半田で接合し、引張り試験を行なった。半
田接合直後の初期接合強度、１５０℃の炉に２４時間放
置した後の強度の２種類についてそれぞれ基板を１０枚
について測定を行なった。初期強度は平均値が４．５ｋ
ｇ、１５０℃×２４ｈｒ放置後は平均値が１．５ｋｇ以
上を合格とする。(2) Adhesive strength 2 mm of conductor paste on a 2.54 cm square alumina substrate
Five square patterns were printed, and after firing at 850 ° C., a tin-plated copper wire having a diameter of 0.65 mm was joined to the conductor portion by Pb—Sn solder containing 37% by weight of lead and the balance tin, and a tensile test was conducted. The initial bonding strength immediately after solder bonding and the strength after being left in a furnace at 150 ° C. for 24 hours were measured for each of 10 substrates. 4.5k average initial strength
After being left for 150 hours at 150 ° C. for 24 hours, an average value of 1.5 kg or more is regarded as acceptable.
【００１８】（３）半田濡れ性 ２．５４ｃｍ角のアルミナ基板に導体ペーストを１０ｍ
ｍ角パータンで印刷し、８５０℃で焼成後導体部にフラ
ックスを滴下し、直径４ｍｍ、高さ２．８５ｍｍの円柱
状に形成された鉛３７重量％、残部錫のＰｂ−Ｓｎ半田
をのせ、該基板を２３０℃の半田浴上に浮かべ、１０秒
後に取り出し、溶融固化した半田の広がり直径を測定し
た。この値が大きいほど半田濡れ性が良いことを示す。
直径５．６ｍｍ以上を合格とする。(3) Solder wettability: 10 m of conductor paste is applied to a 2.54 cm square alumina substrate.
After printing with m-square pattern and firing at 850 ° C., flux is dropped on the conductor part, and 37% by weight of lead formed into a cylindrical shape having a diameter of 4 mm and a height of 2.85 mm, and Pb—Sn solder of the remaining tin are placed, The substrate was floated on a solder bath at 230 ° C., taken out after 10 seconds, and the spread diameter of the melted and solidified solder was measured. The larger this value, the better the solder wettability.
A diameter of 5.6 mm or more is passed.
【００１９】試験結果を表１にまとめて示す。The test results are summarized in Table 1.
【００２０】[0020]
【表１】 [Table 1]
【００２１】表１の結果から、Ｂｉ2 Ｏ3 −ＴｅＯ2溶
融粉砕物中のＴｅＯ2 含有量は１５〜３２モル％とする
必要があること、また、この粉砕物は接着強度と半田濡
れ性の確保の点から、全固形分中に２〜１１重量％の範
囲とする必要があることがわかる。From the results shown in Table 1, it is necessary that the content of TeO 2 in the Bi 2 O 3 -TeO 2 melt pulverized product is 15 to 32 mol%, and that the pulverized product has adhesive strength and solder wettability. From the viewpoint of securing the above, it is understood that it is necessary to set the range of 2 to 11% by weight in the total solid content.
【００２２】[0022]
【発明の効果】本発明によれば、ステインが発生しにく
く、半田付けが容易でしかも基板との接着力の充分な電
極が形成でき、かつ製造時の作業環境上の問題のない導
体ペーストを提供することができる。According to the present invention, a conductive paste which is less likely to cause stains, can be easily soldered, has an electrode having a sufficient adhesive force to a substrate, and has no problem in the working environment during manufacturing can be obtained. Can be provided.
Claims (1)
粉末及びＴｅＯ2 含有率が１５〜３２モル％であるＢｉ
2 Ｏ3 −ＴｅＯ2 溶融粉砕物を含有し、該溶融粉砕物は
ペースト固形分中に２〜１１重量％含有されていること
を特徴とする導体ペースト。1. A composite powder containing silver and palladium, a glass powder and Bi having a TeO 2 content of 15 to 32 mol%.
A conductor paste containing a 2 O 3 -TeO 2 melt pulverized product, wherein the melt pulverized product is contained in an amount of 2 to 11% by weight in the paste solid content.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31857391A JPH05128910A (en) | 1991-11-07 | 1991-11-07 | Conductor paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31857391A JPH05128910A (en) | 1991-11-07 | 1991-11-07 | Conductor paste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05128910A true JPH05128910A (en) | 1993-05-25 |
Family
ID=18100646
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31857391A Pending JPH05128910A (en) | 1991-11-07 | 1991-11-07 | Conductor paste |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05128910A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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-
1991
- 1991-11-07 JP JP31857391A patent/JPH05128910A/en active Pending
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