JP3033852B2 - Resistor and resistor paste composition for aluminum nitride heater - Google Patents
Resistor and resistor paste composition for aluminum nitride heaterInfo
- Publication number
- JP3033852B2 JP3033852B2 JP3063306A JP6330691A JP3033852B2 JP 3033852 B2 JP3033852 B2 JP 3033852B2 JP 3063306 A JP3063306 A JP 3063306A JP 6330691 A JP6330691 A JP 6330691A JP 3033852 B2 JP3033852 B2 JP 3033852B2
- Authority
- JP
- Japan
- Prior art keywords
- resistor
- aluminum nitride
- heater
- paste composition
- resistance
- 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 - Fee Related
Links
Landscapes
- Resistance Heating (AREA)
- Ceramic Products (AREA)
- Glass Compositions (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、窒化アルミニウムヒー
タ用抵抗体及び抵抗ペースト組成物に関し、特に窒化ア
ルミニウム焼結体上にヒータ用の抵抗発熱体としてパタ
ーン形成された抵抗体及び抵抗ペースト組成物に関す
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a resistor and a resist paste composition for an aluminum nitride heater, and more particularly to a resistor and a resist paste composition formed on an aluminum nitride sintered body as a resistive heating element for a heater. About.
【０００２】[0002]
【従来の技術】窒化アルミニウム焼結体は、電気的絶縁
性に優れ、特に非常に高い熱伝導率を持つ材料として、
例えばレーザ素子やマイクロ波送信機用等のハイパワー
ハイブリッドＩＣや、高集積密度のＬＳＩの基板への応
用が有望視されている。また、その高い熱伝導率に加え
て熱膨張率がアルミナの半分以下と小さいので、非常に
高い耐熱衝撃性を有している。この性質を応用すれば優
れたヒータ用構造材として用いることができる。2. Description of the Related Art Aluminum nitride sintered bodies have excellent electrical insulation properties, and in particular, have a very high thermal conductivity.
For example, application to high-power hybrid ICs for laser devices, microwave transmitters, and the like, and high integration density LSI substrates is promising. In addition to the high thermal conductivity, the thermal expansion coefficient is as small as half or less of that of alumina, so that it has very high thermal shock resistance. If this property is applied, it can be used as an excellent heater structural material.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、窒化ア
ルミニウム焼結体をヒータ用途に供する場合、表面に厚
膜印刷法等で抵抗発熱体のパターンを形成しようとして
も、ペーストに含まれるガラスフリット成分が窒化アル
ミニウムを酸化してしまい、その結果として強い金属膜
と基板との接合層が形成されず、高い密着強度が得られ
ない。厚膜ＨＩＣ用導体ペーストまたは抵抗体ペースト
を代用する手段も考えられるが、前者は抵抗値が０．０
５Ω／□未満と小さく、後者は抵抗値が１０Ω／□以上
と大きいので、ヒータ用途として使用するのには難があ
った。したがって、ニクロム線などの発熱体素線を焼結
体の周囲に巻き付ける以外にヒータ用に用いることは不
可能であった。However, when an aluminum nitride sintered body is used for a heater, even if a pattern of a resistance heating element is to be formed on the surface by a thick film printing method or the like, the glass frit component contained in the paste is reduced. The aluminum nitride is oxidized, and as a result, a strong bonding layer between the metal film and the substrate is not formed, and high adhesion strength cannot be obtained. Means for substituting the conductor paste or the resistor paste for the thick film HIC may be considered, but the former has a resistance value of 0.0
Since the resistance value was as small as less than 5 Ω / □ and the resistance value of the latter was as large as 10 Ω / □ or more, it was difficult to use it for heater applications. Therefore, it was impossible to use a heating element wire such as a nichrome wire for a heater other than winding it around the sintered body.
【０００４】本発明は上記問題点を克服し、窒化アルミ
ニウム焼結体への接着強度が大きい抵抗体層を形成し
た、窒化アルミニウムヒータ用抵抗体及び抵抗ペースト
組成物を提供することにある。An object of the present invention is to provide a resistor and a resistor paste composition for an aluminum nitride heater in which a resistor layer having a large adhesive strength to an aluminum nitride sintered body is formed, overcoming the above problems.
【０００５】[0005]
【課題を解決するための手段】本発明者らは上記目的を
達成すべく鋭意研究を重ねた結果、白金、パラジウム、
銀、金の群より選ばれる一種以上の金属粉末及び結晶化
温度が７００℃以上のガラスフリットを配合することに
よって、焼成後の面積抵抗率が０．０５Ω／□以上１０
Ω／□以下での窒化アルミニウム焼結体への接着強度が
大きい抵抗体層及び抵抗ペースト組成物を形成すること
ができることを見出し、本発明に到達した。Means for Solving the Problems The present inventors have made intensive studies to achieve the above object, and as a result, platinum, palladium,
By mixing at least one metal powder selected from the group consisting of silver and gold and a glass frit having a crystallization temperature of 700 ° C. or more, the area resistivity after firing is 0.05 Ω / □ or more.
The present inventors have found that it is possible to form a resistor layer and a resist paste composition having a large adhesive strength to an aluminum nitride sintered body at Ω / □ or less, and have reached the present invention.
【０００６】[0006]
【作用】本発明に用いる金属粉末としては、白金、パラ
ジウム、銀、金の群より選ばれる一種以上の金属粉末で
ある。二種以上の金属を使用する場合は、単体の混合物
の他、予め合金化された粉末を利用してもよい。また、
抵抗温度係数の向上や焼結の促進のために、他の白金属
元素等を少量添加しても差し支えない。The metal powder used in the present invention is at least one metal powder selected from the group consisting of platinum, palladium, silver and gold. When two or more metals are used, a pre-alloyed powder may be used in addition to a single mixture. Also,
In order to improve the temperature coefficient of resistance and promote sintering, a small amount of another white metal element or the like may be added.
【０００７】白金、パラジウム、銀、金はすべて高温下
での耐酸化性が高く、ヒータ用発熱抵抗体として用いた
時の経時劣化が少ない。これらの金属の配合割合は任意
であり、目的の抵抗温度特性や面積抵抗率を勘案して適
宜選択する。結晶化温度が７００℃以上の結晶化ガラス
フリットとしては、例えばＳｉＯ2２５−３０ｗｔ％、
Ａｌ2 Ｏ3 ７−１５ｗｔ％、ＣａＯ１５−２４ｗｔ％、
ＴｉＯ2 ８−１５ｗｔ％、ＺｎＯ２０−３０ｗｔ％、Ｂ
2 Ｏ3 ０−５ｗｔ％の割合で含有するものが挙げられ
る。この結晶化ガラスフリットの結晶化温度が７００℃
に満たないと、高温でのヒータ作動中に溶融または軟化
してしまう恐れがあり、実用に供することができない。
結晶化ガラスフリットの金属粉末に対する配合量には特
に制約はなく、配合量に対して面積抵抗率が指数関数的
に増加するので、目的とする面積抵抗率によって決定さ
れる。[0007] Platinum, palladium, silver, and gold all have high oxidation resistance at high temperatures and have little deterioration over time when used as a heating resistor for a heater. The mixing ratio of these metals is arbitrary, and is appropriately selected in consideration of the desired resistance temperature characteristics and the sheet resistivity. As a crystallized glass frit having a crystallization temperature of 700 ° C. or more, for example, SiO 2 25-30 wt%,
Al 2 O 3 7-15 wt%, CaO 15-24 wt%,
TiO 2 8-15 wt%, ZnO 20-30 wt%, B
Those containing at a rate of 0-5 wt% of 2 O 3 are exemplified. The crystallization temperature of this crystallized glass frit is 700 ° C.
If the temperature is lower than the above range, the heater may be melted or softened during the operation of the heater at a high temperature, and cannot be put to practical use.
There is no particular limitation on the amount of the crystallized glass frit with respect to the metal powder, and the sheet resistivity increases exponentially with respect to the compounding amount.
【０００８】面積抵抗率は０．０５Ω／□未満でも１０
Ω／□超でもヒータ用発熱抵抗体として用いるには不適
なのでこの範囲に限定した。この範囲に抵抗値を収める
ためには、金属粉末に対する結晶化ガラスフリットの量
を増減する。本発明組成物において、金属粉末並びに結
晶化ガラス粉末の他に結晶化温度の調整や密着強度をさ
らに向上させる目的でＺｎＯ、ＢｉＯ3 、ＣｄＯ、Ｓｂ
2 Ｏ 5 、Ｓｂ2 Ｏ3 、Ｖ2 Ｏ5 、Ｃｒ2 Ｏ3 、Ｔｉ
Ｏ2、ＺｒＯ2 、Ｎｂ2 Ｏ5 等の無機酸化物を配合して
も差し支えない。これら無機酸化物の添加量には特に制
限はないが、金属粉末１００重量部に対して２０重量部
以下の範囲で添加すると好適である。[0008] Even if the sheet resistivity is less than 0.05Ω / □, it is 10
Not suitable for use as a heating resistor for heaters even at Ω / □ or more
Therefore, it was limited to this range. Keep the resistance within this range
To determine the amount of crystallized glass frit relative to the metal powder
Increase or decrease. In the composition of the present invention, the metal powder and the binder
In addition to the crystallized glass powder, adjust the crystallization temperature and adjust the adhesion strength.
ZnO, BiO for the purpose of further improvingThree , CdO, Sb
Two O Five , SbTwo OThree , VTwo OFive , CrTwo OThree , Ti
OTwo, ZrOTwo , NbTwo OFive Blending inorganic oxides such as
No problem. The amount of these inorganic oxides added is particularly limited.
20 parts by weight for 100 parts by weight of metal powder
It is preferable to add in the following range.
【０００９】[0009]
【実施例】以下に実施例を挙げて本発明の詳細を説明す
るが、もとより本発明は実施例の範囲に限定されるもの
ではない。表１、表２に示す配合にしたがって、各種金
属粉末と結晶化ガラスを有機ビヒクルと共に三本ロール
機にて混練・分散を行ってペーストを得た。ただし、金
属粉末としてはすべて平均粒径０．１〜１．５μｍのも
のを用いた。ただし、表中のガラス粉Ａは結晶化温度７
５０℃のＺｎＯ−Ｂ2 Ｏ 3−ＳｉＯ2 系、ガラス粉Ｂ、
Ｃはそれぞれ結晶化温度８００℃、８７５℃のＡｌ2 Ｏ
3−ＣａＯ−ＳｉＯ 2 系の結晶化ガラスフリットであ
る。このペーストを川崎製鉄製窒化アルミニウム基板上
に印刷し、空気中ピーク温度９５０℃、ピーク温度保持
時間７分、入口から出口まで４０分でベルト炉で焼成し
た。ベルト炉には光洋リンドバーグ社製パイロットII型
ベルト炉を用いた。The present invention will be described below in detail with reference to examples.
However, the present invention is naturally limited to the scope of the examples.
is not. Various types of gold were used according to the formulations shown in Tables 1 and 2.
Three rolls of genus powder and crystallized glass with organic vehicle
The paste was obtained by kneading and dispersing in a machine. However, gold
All powders of the genus have a mean particle size of 0.1 to 1.5 μm.
Was used. However, the glass powder A in the table had a crystallization temperature of 7
ZnO-B at 50 ° CTwo OThree-SiOTwo System, glass powder B,
C is a crystallization temperature of 800 ° C. and 875 ° C., respectively.Two O
Three-CaO-SiO Two Crystallized glass frit
You. This paste is applied on an aluminum nitride substrate made by Kawasaki Steel.
Printed on air, peak temperature in air 950 ° C, peak temperature maintained
Firing in a belt furnace in 7 minutes, 40 minutes from the entrance to the exit
Was. Pilot type II manufactured by Koyo Lindberg Co., Ltd.
A belt furnace was used.
【００１０】基板上には２ｍｍ×２ｍｍのパッドを１０
個形成し、焼成終了後無電解Ｎｉメッキを施した後６／
４ハンダ浴中に基板を５秒間浸漬し、それぞれのパッド
上に０．８ｍｍのスズ被覆銅線をハンダ付けし、９０度
ピール試験を行い、接着強度を測定した。これらの結果
を表１、表２に示した。抵抗値の値は基板上に形成した
長さ１７１ｍｍ、幅０．４ｍｍのパターンの両端を電子
式抵抗計で測定した。また、このパターンに１００Ｗの
消耗電力になるように電流を２０００時間通電し、その
後の抵抗値の変化を調べた。A 2 mm × 2 mm pad is formed on the substrate by 10
After forming the individual pieces and performing the electroless Ni plating after the firing,
The substrate was immersed in a 4 solder bath for 5 seconds, a 0.8 mm tin-coated copper wire was soldered on each pad, and a 90 degree peel test was performed to measure the adhesive strength. The results are shown in Tables 1 and 2. The resistance value was measured at both ends of a pattern having a length of 171 mm and a width of 0.4 mm formed on the substrate by using an electronic resistance meter. In addition, a current was applied to this pattern for 2000 hours so as to consume 100 W of power, and a change in resistance value after that was examined.
【００１１】これらの結果から分かるように本発明の抵
抗体は平均４ｋｇ／２ｍｍ□以上と強く、また通電後の
抵抗値の劣化も少なく、実用的であることが分かる。As can be seen from these results, the resistor of the present invention is practical, having a strong average of 4 kg / 2 mm square or more, and has little deterioration of the resistance value after energization.
【００１２】[0012]
【表１】 [Table 1]
【００１３】[0013]
【表２】 [Table 2]
【００１４】[0014]
【発明の効果】本発明による窒化アルミニウムヒータ用
抵抗体は窒化アルミニウム焼結体の表面に主として印刷
によって塗布し焼成することにより、接着強度が大きい
抵抗体として形成することができるもので、その工業的
利用価値は大である。Industrial Applicability The resistor for an aluminum nitride heater according to the present invention can be formed as a resistor having a large adhesive strength by coating and firing mainly on the surface of an aluminum nitride sintered body by printing. The value of public use is great.
───────────────────────────────────────────────────── フロントページの続き (73)特許権者 000224798 同和鉱業株式会社 東京都千代田区丸の内１丁目８番２号 (72)発明者 中野 正 千葉市川崎町１番地 川崎製鉄株式会社 技術研究本部内 (72)発明者 佐藤 弘志 千葉市川崎町１番地 川崎製鉄株式会社 技術研究本部内 (72)発明者 熊谷 正人 千葉市川崎町１番地 川崎製鉄株式会社 技術研究本部内 (72)発明者 船橋 敏彦 千葉市川崎町１番地 川崎製鉄株式会社 技術研究本部内 (72)発明者 小松 政男 東京都板橋区赤塚新町３−34−２−101 (72)発明者 佐伯 周二 大津市陽明町８−７ (72)発明者 岡田 駿 逗子市沼間５丁目 765−120 (72)発明者 末広 雅利 京都市西京区川島粟田町50−８ (56)参考文献 特開 平３−47878（ＪＰ，Ａ) 特開 昭63−81787（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C04B 41/86 C03C 8/18 C04B 35/58 H05B 3/14 ──────────────────────────────────────────────────の Continued on the front page (73) Patent holder 000224798 Dowa Mining Co., Ltd. 1-8-2 Marunouchi, Chiyoda-ku, Tokyo (72) Inventor Tadashi Nakano 1 Kawasaki-cho, Chiba-shi Kawasaki Steel Corporation Research and Development Headquarters (72) Inventor Hiroshi Sato 1 Kawasaki-cho, Chiba-shi Kawasaki Steel Corporation, Technology Research Division (72) Inventor Masato Kumagai 1-Kawasaki-cho, Chiba City Kawasaki Steel Corporation Technical Research Division (72) Inventor Toshihiko Funabashi Chiba No. 1 Ichikawasakicho Kawasaki Steel Corporation (72) Inventor Masao Komatsu 3-34-2-101 Akatsuka Shinmachi, Itabashi-ku, Tokyo (72) Inventor Shuji Saeki 8-7 Yomeicho, Otsu-shi (72) Inventor Shun Okada 5-765-120 Numa, Zushi City (72) Inventor Masatoshi Suehiro 50-8 Kawashima Awatacho, Nishikyo-ku, Kyoto-shi (56) References 47878 (JP, A) JP Akira 63-81787 (JP, A) (58 ) investigated the field (Int.Cl. 7, DB name) C04B 41/86 C03C 8/18 C04B 35/58 H05B 3/14
Claims (2)
れる一種以上の金属粉末及び結晶化温度が７００℃以上
のガラスフリットからなり、焼成後の面積抵抗率が０．
０５Ω／□以上１０Ω／□以下であることを特徴とする
窒化アルミニウムヒータ用抵抗体。1. A material comprising at least one metal powder selected from the group consisting of platinum, palladium, silver and gold, and a glass frit having a crystallization temperature of 700 ° C. or more, and having a sheet resistivity of 0.2 after firing.
A resistor for an aluminum nitride heater, having a resistance of from 05 Ω / □ to 10 Ω / □.
れる一種以上の金属粉末及び結晶化温度が７００℃以上
のガラスフリットからなり、焼成後の面積抵抗率が０．
０５Ω／□以上１０Ω／□以下であることを特徴とする
窒化アルミニウム用抵抗ペースト組成物。2. A powder comprising at least one metal powder selected from the group consisting of platinum, palladium, silver and gold, and a glass frit having a crystallization temperature of 700 ° C. or more, and having a sheet resistivity of 0.2 after firing.
A resistance paste composition for aluminum nitride, having a resistance of from 05 Ω / □ to 10 Ω / □.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3063306A JP3033852B2 (en) | 1991-03-27 | 1991-03-27 | Resistor and resistor paste composition for aluminum nitride heater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3063306A JP3033852B2 (en) | 1991-03-27 | 1991-03-27 | Resistor and resistor paste composition for aluminum nitride heater |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04300249A JPH04300249A (en) | 1992-10-23 |
| JP3033852B2 true JP3033852B2 (en) | 2000-04-17 |
Family
ID=13225478
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3063306A Expired - Fee Related JP3033852B2 (en) | 1991-03-27 | 1991-03-27 | Resistor and resistor paste composition for aluminum nitride heater |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3033852B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006068121A1 (en) * | 2004-12-20 | 2006-06-29 | Matsushita Electric Industrial Co., Ltd. | Strain sensor and method for manufacture thereof |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0747332B1 (en) * | 1994-12-01 | 2001-09-12 | Kabushiki Kaisha Toshiba | Aluminum nitride sinter and process for producing the same |
| JP2001203066A (en) * | 1999-05-07 | 2001-07-27 | Ibiden Co Ltd | Hot plate and conductive paste |
| JP4021139B2 (en) * | 1999-09-30 | 2007-12-12 | 東京エレクトロン株式会社 | Heat treatment apparatus and heat treatment method |
| EP1274280A1 (en) | 2000-04-14 | 2003-01-08 | Ibiden Co., Ltd. | Ceramic heater |
| KR100794987B1 (en) * | 2004-12-14 | 2008-01-16 | 김형우 | A heating apparatus of wafer deposition substrate |
| WO2008081766A1 (en) * | 2006-12-25 | 2008-07-10 | Rohm Co., Ltd. | Fixing heater and method for manufacturing the same |
| JP2008159427A (en) * | 2006-12-25 | 2008-07-10 | Rohm Co Ltd | Heater |
| US7659220B1 (en) * | 2008-12-03 | 2010-02-09 | Osram Sylvania Inc. | Sealing composition for sealing aluminum nitride and aluminum oxynitride ceramics |
| JP5662361B2 (en) * | 2012-02-09 | 2015-01-28 | 京都エレックス株式会社 | Resistor paste for ceramic substrate heater and ceramic substrate heater |
-
1991
- 1991-03-27 JP JP3063306A patent/JP3033852B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006068121A1 (en) * | 2004-12-20 | 2006-06-29 | Matsushita Electric Industrial Co., Ltd. | Strain sensor and method for manufacture thereof |
| US7882747B2 (en) | 2004-12-20 | 2011-02-08 | Panasonic Corporation | Strain sensor and method for manufacture thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04300249A (en) | 1992-10-23 |
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