JPH0945131A - Copper paste - Google Patents
Copper pasteInfo
- Publication number
- JPH0945131A JPH0945131A JP21134195A JP21134195A JPH0945131A JP H0945131 A JPH0945131 A JP H0945131A JP 21134195 A JP21134195 A JP 21134195A JP 21134195 A JP21134195 A JP 21134195A JP H0945131 A JPH0945131 A JP H0945131A
- Authority
- JP
- Japan
- Prior art keywords
- copper
- pts
- weight
- parts
- adhesion strength
- 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
Abstract
Description
【０００１】[0001]
【産業上の利用分野】この発明は、抵抗体等の特性を変
化させる事無く電気的接合部を形成することができる銅
ペーストに関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a copper paste which can form an electrical joint without changing the characteristics of a resistor or the like.
【０００２】[0002]
【従来の技術】一般に、銅ペーストの密着強度を高める
ために添加物を加えることが種々開示されている。例え
ば、特開平３−２２３０６号公報では二酸化亜鉛ＺｎＯ
2、又は二酸化チタンＴｉＯ2粉を添加する事が、特開平
２−２６３７３１号公報、特公平2-55460号公報では酸
化チタンを添加する事が、また、特開昭６０−７０７４
６号公報には、タングステンＷ、レニウムＲｅ、モリブ
デンＭｏを添加する事が示されている。2. Description of the Related Art In general, it has been disclosed that various additives are added to enhance the adhesion strength of copper paste. For example, in JP-A-3-22306, zinc dioxide ZnO is used.
2 , or addition of titanium dioxide TiO 2 powder, addition of titanium oxide in JP-A-2-263731 and JP-B-2-55460, and JP-A-60-7074.
Japanese Patent Publication No. 6 discloses that tungsten W, rhenium Re and molybdenum Mo are added.
【０００３】プリント配線板やＩＣ等では抵抗体等の機
械部品と導体とをペースト焼成体から形成する事が行わ
れている。抵抗用ペーストには酸化ルテニウムＲｕＯ2
が含有されるため、抵抗ペースト焼成体の上に重ねて銅
ペーストを施して約９００℃で焼成すると、抵抗体と銅
導体との接合部で酸化ルテニウムＲｕＯ2の欠之層が生
成されて抵抗値が変化してしまう。そのため、この様な
場合は約６００℃という通常より低い温度で焼成せざる
を得ない。この場合、抵抗値の変化は生じないものの、
銅導体と基板との密着強度が充分とは言えない。In printed wiring boards, ICs, etc., mechanical parts such as resistors and conductors are formed from a paste fired body. Ruthenium oxide RuO 2 is used for the resistor paste.
Therefore, when copper paste is applied on the fired resistor paste and fired at about 900 ° C., a missing layer of ruthenium oxide RuO 2 is generated at the junction between the resistor and the copper conductor, and The value changes. Therefore, in such a case, there is no choice but to fire at a temperature lower than usual, which is about 600 ° C. In this case, although the resistance value does not change,
It cannot be said that the adhesion strength between the copper conductor and the substrate is sufficient.
【０００４】[0004]
【発明が解決しようとする課題】そこで、この発明は、
６００℃前後の焼成温度でも銅導体と基板との密着強度
が得られる様にしようとするものである。即ち、この発
明は、低温焼成しても基板との間の充分な密着強度が得
られる銅ペーストを提供する事を目的とする。SUMMARY OF THE INVENTION Therefore, the present invention
It is intended to obtain adhesion strength between the copper conductor and the substrate even at a firing temperature of about 600 ° C. That is, an object of the present invention is to provide a copper paste which can obtain a sufficient adhesion strength with a substrate even if it is fired at a low temperature.
【０００５】[0005]
【課題を解決するための手段】この発明の目的は、溶剤
に樹脂を溶解させたビヒクルと、銅粉末と、ガラスフリ
ットと、有機金属とを含有する銅ペーストによって達成
される。The object of the present invention is achieved by a copper paste containing a vehicle in which a resin is dissolved in a solvent, copper powder, glass frit, and an organic metal.
【０００６】この発明の目的は、有機金属は、銅の脂肪
酸、鉛の脂肪酸、及びホウ素の脂肪酸のうちいずれか一
つが選ばれることを特徴とする請求項１の銅ペーストに
よっても達成される。The object of the present invention is also achieved by the copper paste according to claim 1, wherein the organic metal is selected from the group consisting of copper fatty acid, lead fatty acid and boron fatty acid.
【０００７】[0007]
【作用】銅ペースト中に含有される有機金属は、有機物
であるので銅粉との分散性が良好であり、かつ焼成され
た有機金属は基板とのアンカーの役割をはたし、焼成銅
導体を能く基板に保持する。[Function] Since the organic metal contained in the copper paste is an organic substance, it has good dispersibility with the copper powder, and the calcined metal serves as an anchor with the substrate, and the calcined copper conductor Is effectively held on the substrate.
【０００８】有機金属として、銅の脂肪酸、鉛の脂肪
酸、又はホウ素の脂肪酸を用いた場合には、アルミナ基
板との親和性が良く、良好な密着強度が得られる。When a fatty acid of copper, a fatty acid of lead, or a fatty acid of boron is used as the organic metal, the affinity with the alumina substrate is good and good adhesion strength is obtained.
【０００９】[0009]
【実施例】銅ペーストは通常、溶剤に樹脂を溶解させた
ビヒクルと、銅粉末と、ガラスフリットと、酸化銅を混
合して製造する。ここで、樹脂としては、エチルセルロ
ーズ、ポリイソブナルメタクリレート等が用いられ、溶
剤としてはターピネオイル、ブチルカルビトールアセテ
ート、２，２，４トリメチルペンタンジオールモノイソ
ブチレート等が用いられる。EXAMPLE A copper paste is usually produced by mixing a vehicle in which a resin is dissolved in a solvent, copper powder, glass frit, and copper oxide. Here, as the resin, ethyl cellulose, polyisobunal methacrylate, etc. are used, and as the solvent, terpineol oil, butyl carbitol acetate, 2,2,4 trimethylpentanediol monoisobutyrate, etc. are used.
【００１０】次に、比表面積０．４ｍ2／ｇ、タップ密
度４．２ｇ／ｃｃの銅粉末Ａと、比表面積１．８ｍ2／
ｇ、タップ密度４．３ｇ／ｃｃの銅粉末Ｂと各材料とを
混合した銅ペーストの実施例と比較例について述べる。Next, copper powder A having a specific surface area of 0.4 m 2 / g and a tap density of 4.2 g / cc and a specific surface area of 1.8 m 2 /
An example and a comparative example of a copper paste in which copper powder B having a g and a tap density of 4.3 g / cc and each material are mixed will be described.
【００１１】この際製造された銅ペーストは、２００メ
ッシュ或いは３２５メッシュのスクリーンを用いて９６
％アルミナ基板上に印刷され乾燥されて、６００℃３０
分、ピーク温度時間５分の温度プロファイルで窒素雰囲
気焼成されて評価された。評価は、２ｍｍ×２ｍｍのパ
ッドとアルミナ基板との密着強度をピール引張法で測定
した。測定は焼成後の初期密着強度（Ｋｇ）とヒートサ
イクル後の密着強度（Ｋｇ）とを測定し、ヒートサイク
ルはー５５℃と＋１２５℃各３０分を１００サイクルで
行った。At this time, the copper paste produced is 96 by using a screen of 200 mesh or 325 mesh.
% Printed on alumina substrate, dried, 600 ° C 30
Min, peak temperature time 5 minutes The temperature profile was evaluated by firing in a nitrogen atmosphere. For the evaluation, the adhesion strength between the 2 mm × 2 mm pad and the alumina substrate was measured by the peel tension method. The measurement was carried out by measuring the initial adhesion strength (Kg) after firing and the adhesion strength (Kg) after the heat cycle, and the heat cycle was carried out at −55 ° C. and + 125 ° C. for 30 minutes each for 100 cycles.
【００１２】[0012]
【実施例１】銅粉末Ａ６０重量部と銅粉末Ｂ４０重量
部、ＰｂＯ2 ７０％，ＳｉＯ2 ５％，Ｂ2Ｏ3 １５
％，ＺｎＯ １０％からなるガラスフリット８重量部、
酸化銅１２重量部、エチルセルロース１．５重量部、
２．２．４トリメチルペンタンジオルモノイソブチレー
ト１０重量部、及び有機金属としてオクチル酸鉛（鉛含
有率１５％）を１重量部を混合分散させた銅ペーストを
２００メッシュスクリーンを用いてアルミナ基板上に印
刷焼成後、評価した所、初期の密着強度は３．７０Ｋ
ｇ、ヒートサイクル１００サイクル後の密着強度は２．
３０ｋｇであった。Example 1 60 parts by weight of copper powder A and 40 parts by weight of copper powder B, PbO 2 70%, SiO 2 5%, B 2 O 3 15
%, Glass frit consisting of 10% ZnO 8 parts by weight,
Copper oxide 12 parts by weight, ethyl cellulose 1.5 parts by weight,
2.2.4 10 parts by weight of trimethylpentanediolmonoisobutyrate and 1 part by weight of lead octylate (lead content 15%) as an organic metal were mixed and dispersed in a copper paste using a 200 mesh screen to form an alumina substrate. After printing and baking on the surface, the evaluation showed that the initial adhesion strength was 3.70K.
g, the adhesion strength after 100 heat cycles is 2.
It was 30 kg.
【００１３】[0013]
【実施例２】銅粉末Ａ６０重量部と銅粉末Ｂ４０重量
部、ＰｂＯ2 ７０％，ＳｉＯ2 ５％，Ｂ2Ｏ3 １５
％，ＺｎＯ １０％からなるガラスフリット８重量部、
酸化銅１２重量部、エチルセルローズ １．５重量部、
２，２，４トリメチルペンタンジオルモノイソブチレー
ト１０重量部、及び有機金属としてナフテン酸銅（銅含
有率５％）を１重量部混合分散させた銅ペーストを２０
０メッシュスクリーンを用いてアルミナ基板上に印刷し
て焼成後評価した所、初期の密着強度は３．４１Ｋｇ、
ヒートサイクル１００サイクル後の密着強度は２．５９
Ｋｇであった。Example 2 60 parts by weight of copper powder A and 40 parts by weight of copper powder B, PbO 2 70%, SiO 2 5%, B 2 O 3 15
%, Glass frit consisting of 10% ZnO 8 parts by weight,
Copper oxide 12 parts by weight, ethyl cellulose 1.5 parts by weight,
20 parts by weight of a copper paste prepared by mixing and dispersing 10 parts by weight of 2,2,4 trimethylpentanediolmonoisobutyrate and 1 part by weight of copper naphthenate (copper content 5%) as an organic metal.
When printed on an alumina substrate using a 0 mesh screen and evaluated after firing, the initial adhesion strength was 3.41 Kg,
Adhesion strength after heat cycle 100 cycles is 2.59
Kg.
【００１４】[0014]
【実施例３】銅粉末Ａ７５重量部と銅粉末Ｂ２５重量
部、ＰｂＯ2 ７６．５％，ＳｉＯ2５．８％，Ｂ2Ｏ3
１２．７％，ＺｎＯ５．０％からなるガラスフリット８
重量部、酸化銅１５重量部、エチルセルローズ３重量
部、２，２，４トリメチルペンタンジオルモノイソブチ
レート１４重量部、及び有機金属としてオクチル酸ホウ
素（ホウ素含有率６．５％）を２重量部混合分散させた
銅ペーストを２００メッシュスクリーンを用いてアルミ
ナ基板上に印刷して焼成後評価した所、初期の密着強度
は３．５２Ｋｇ、ヒートサイクル１００サイクル後の密
着強度は２．４０Ｋｇであった。Example 3 Copper powder A 75 parts by weight and copper powder B 25 parts by weight, PbO 2 76.5%, SiO 2 5.8%, B 2 O 3
Glass frit 8 composed of 12.7% and ZnO 5.0%
Parts by weight, 15 parts by weight of copper oxide, 3 parts by weight of ethyl cellulose, 14 parts by weight of 2,2,4 trimethylpentanediolmonoisobutyrate, and 2 parts by weight of octyl borate (boron content 6.5%) as an organic metal. Part of the copper paste mixed and dispersed was printed on an alumina substrate using a 200 mesh screen and evaluated after firing. The initial adhesion strength was 3.52 kg, and the adhesion strength after 100 heat cycles was 2.40 Kg. It was
【００１５】[0015]
【実施例４】銅粉末Ａ７５重量部と銅粉末Ｂ２５重量
部、ＰｂＯ2 ６６．３％，ＳｉＯ2１２．９％，Ｂ2Ｏ3
１５．８％，ＺｎＯ ５．０％からなるガラスフリッ
ト８重量部、酸化銅１５重量部、エチルセルローズ３重
量部、２，２，４トリメチルペンタンジオルモノイソブ
チレート１４重量部、及び有機金属としてオクチル酸ホ
ウ素（ホウ素含有率６．５％）を２重量部を混合分散さ
せた銅ペーストを２００メッシュスクリーンを用いてア
ルミナ基板上に印刷し、焼成後に評価した所、初期の密
着強度は３．６９Ｋｇ、ヒートサイクル１００サイクル
後の密着強度は２．４２Ｋｇであった。Example 4 Copper powder A 75 parts by weight and copper powder B 25 parts by weight, PbO 2 66.3%, SiO 2 12.9%, B 2 O 3
8 parts by weight of glass frit consisting of 15.8% and 5.0% ZnO, 15 parts by weight of copper oxide, 3 parts by weight of ethyl cellulose, 14 parts by weight of 2,2,4 trimethylpentanediolmonoisobutyrate, and as an organic metal When a copper paste in which 2 parts by weight of boron octylate (boron content 6.5%) was mixed and dispersed was printed on an alumina substrate using a 200 mesh screen and evaluated after firing, the initial adhesion strength was 3. The adhesion strength was 69 kg and 2.42 kg after 100 heat cycles.
【００１６】[0016]
【比較例１】銅粉末Ａ６０重量部と銅粉末Ｂ４０重量
部、ＰｂＯ2 ７０％，ＳｉＯ2 ５％，Ｂ2Ｏ3 １５
％，ＺｎＯ １０％からなるガラスフリット８重量部、
酸化銅１２重量部、エチルセルローズ１．５重量部、及
び２．２．４トリメチルペンタンジオルモノイソブチレ
ート１１重量部を混合分散させた従来と同様な銅ペース
トを３２５メッシュスクリーンを用いてアルミナ基板上
に印刷して焼成後評価すると、初期の密着強度は３．１
１Ｋｇ、ヒートサイクル１００サイクル後の密着強度は
２．０２Ｋｇであった。Comparative Example 1 60 parts by weight of copper powder A and 40 parts by weight of copper powder B, PbO 2 70%, SiO 2 5%, B 2 O 3 15
%, Glass frit consisting of 10% ZnO 8 parts by weight,
An alumina substrate was prepared by using a 325 mesh screen and using the same copper paste as the conventional one in which 12 parts by weight of copper oxide, 1.5 parts by weight of ethyl cellulose, and 11 parts by weight of 2.2.4 trimethylpentanediolmonoisobutyrate were mixed and dispersed. When printed on the above and evaluated after firing, the initial adhesion strength was 3.1.
The adhesion strength after 100 cycles of 1 kg and the heat cycle was 2.02 kg.
【００１７】この値を実施例１と比較してみるとこの発
明による実施例１では初期の密着強度３．１１Ｋｇから
３．７０Ｋｇに改善され、約１９％向上ヒートサイクル
１００サイクル後の値は２．０２Ｋｇから２．３０Ｋｇ
と約１４％向上していることがわかる。Comparing this value with Example 1, in Example 1 according to the present invention, the initial adhesion strength was improved from 3.11 Kg to 3.70 Kg, which was improved by about 19% and the value after 100 heat cycles was 2 From 0.02 Kg to 2.30 Kg
It can be seen that the improvement is about 14%.
【００１８】[0018]
【比較例２】銅粉末Ａ７５重量部と銅粉末Ｂ２５重量
部、ＰｂＯ2 ６６．３％，ＳｉＯ2１２．９％，Ｂ2Ｏ3
１５．８％，ＺｎＯ ５．０％からなるガラスフリッ
ト８重量部、酸化銅１５重量部、エチルセルロース３重
量部、２．２．４トリメチルペンタンジオルモノイソブ
チレート１６重量部を混合分散させた銅ペーストを３２
５メッシュスクリーンを用いてアルミナ基板上に印刷し
て焼成後に評価すると、初期の密着強度は３．３６Ｋ
ｇ、ヒートサイクル１００サイクル後の密着強度は１．
８９Ｋｇであった。Comparative Example 2 75 parts by weight of copper powder A and 25 parts by weight of copper powder B, PbO 2 66.3%, SiO 2 12.9%, B 2 O 3
Copper in which 8 parts by weight of glass frit consisting of 15.8% and 5.0% ZnO, 15 parts by weight of copper oxide, 3 parts by weight of ethyl cellulose, and 16 parts by weight of 2.2.4 trimethylpentanediolmonoisobutyrate are mixed and dispersed. 32 paste
When printed on an alumina substrate using a 5 mesh screen and evaluated after firing, the initial adhesion strength is 3.36K.
g, the adhesion strength after 100 heat cycles is 1.
It was 89 kg.
【００１９】これらの密着強度の値を実施例４と比較し
てみると、初期の密着強度が３．３６Ｋｇから３．６９
Ｋｇに改善され、約１０％向上し、ヒートサイクル１０
０サイクル後の密着強度は、１．８９Ｋｇから２．４２
Ｋｇと約２８％向上している。Comparing these adhesion strength values with those of Example 4, the initial adhesion strength was 3.36 Kg to 3.69.
Improved to Kg, improved about 10%, heat cycle 10
Adhesion strength after 0 cycles is from 1.89 Kg to 2.42
It is about 28% higher than Kg.
【００２０】上記両比較例より、有機金属を含有させた
この発明による銅ペーストの実施例が、従来組成の銅ペ
ーストに比較して良好な密着強度をもたらすことがわか
る。From the above two comparative examples, it can be seen that the examples of the copper paste according to the present invention containing an organic metal provide good adhesion strength as compared with the copper paste of the conventional composition.
【００２１】[0021]
【発明の効果】この発明による銅ペーストによれば、有
機金属が含有されているため、この有機金属が印刷焼成
後には基板に対するアンカーとして作用するので、６０
０℃程度の温度での焼成においても良好な密着強度をも
たらすものとなる。Since the copper paste according to the present invention contains an organic metal, the organic metal acts as an anchor for the substrate after printing and baking.
Good adhesion strength is obtained even when firing at a temperature of about 0 ° C.
【００２２】有機金属として、銅の脂肪酸、鉛の脂肪
酸、及びホウ素の脂肪酸のいずれかを用いる場合には、
特にアルミナ基板との密着強度が良好となる。When any of copper fatty acid, lead fatty acid and boron fatty acid is used as the organic metal,
In particular, the adhesion strength with the alumina substrate is improved.
Claims (2)
粉末と、ガラスフリットと、有機金属とを含有する銅ペ
ースト。1. A copper paste containing a vehicle in which a resin is dissolved in a solvent, copper powder, glass frit, and an organic metal.
びホウ素の脂肪酸のうちのいずれか一つが選ばれる事を
特徴とする請求項１の銅ペースト。2. The copper paste according to claim 1, wherein the organic metal is selected from the group consisting of copper fatty acid, lead fatty acid and boron fatty acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21134195A JPH0945131A (en) | 1995-07-28 | 1995-07-28 | Copper paste |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21134195A JPH0945131A (en) | 1995-07-28 | 1995-07-28 | Copper paste |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0945131A true JPH0945131A (en) | 1997-02-14 |
Family
ID=16604366
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21134195A Pending JPH0945131A (en) | 1995-07-28 | 1995-07-28 | Copper paste |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0945131A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7276325B2 (en) | 2003-02-14 | 2007-10-02 | E.I. Dupont De Nemours And Company | Electrode-forming composition for field emission type of display device, and method using such a composition |
-
1995
- 1995-07-28 JP JP21134195A patent/JPH0945131A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7276325B2 (en) | 2003-02-14 | 2007-10-02 | E.I. Dupont De Nemours And Company | Electrode-forming composition for field emission type of display device, and method using such a composition |
| US7303854B2 (en) | 2003-02-14 | 2007-12-04 | E.I. Du Pont De Nemours And Company | Electrode-forming composition for field emission type of display device, and method using such a composition |
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