JPH08119720A - Alumina ceramic and its production - Google Patents
Alumina ceramic and its productionInfo
- Publication number
- JPH08119720A JPH08119720A JP6274231A JP27423194A JPH08119720A JP H08119720 A JPH08119720 A JP H08119720A JP 6274231 A JP6274231 A JP 6274231A JP 27423194 A JP27423194 A JP 27423194A JP H08119720 A JPH08119720 A JP H08119720A
- Authority
- JP
- Japan
- Prior art keywords
- conductor
- alumina
- temperature
- ceramics
- purity
- 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.)
- Withdrawn
Links
Classifications
-
- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K1/00—Printed circuits
- H05K1/02—Details
- H05K1/09—Use of materials for the conductive, e.g. metallic pattern
- H05K1/092—Dispersed materials, e.g. conductive pastes or inks
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、セラミックス及びその
製造方法に関し、特に導体を内蔵するアルミナセラミッ
クス及びその製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to ceramics and a method for manufacturing the same, and more particularly to alumina ceramics containing a conductor and a method for manufacturing the same.
【０００２】[0002]
【従来の技術】セラミックスは高い絶縁性を有している
ため、その特性を生かして電気部品としてＩＣ基板の
他、点火プラグ、ヒータ、静電チャック等に利用されて
いる。これら電気部品の多くはセラミックス中に導体が
内蔵されている。利用されているセラミックスの中で
は、安価であるなどの利点からアルミナセラミックスが
現在最も広く使われている。このアルミナセラミックス
に用いる導体には、ＷやＭｏなどの金属が使われてい
る。ＷやＭｏなどが使われているのは、アルミナセラミ
ックスの焼成温度が１５００℃以上と高いため、高融点
の金属が必要だからである。2. Description of the Related Art Since ceramics have a high insulating property, they are utilized as electric parts in IC plugs, spark plugs, heaters, electrostatic chucks, etc. by taking advantage of their characteristics. In many of these electric parts, a conductor is built in ceramics. Among the ceramics used, alumina ceramics is currently most widely used because it is inexpensive. A metal such as W or Mo is used for the conductor used for the alumina ceramics. W and Mo are used because the firing temperature of alumina ceramics is as high as 1500 ° C. or higher, so that a metal having a high melting point is required.
【０００３】ところが、これら金属は酸化雰囲気中で焼
成すると酸化され、導電性がなくなるため、非酸化雰囲
気中で焼成を行う必要があった。この焼成は、１０００
℃以上の温度での脱バインダー工程を経た後、通常水分
を含んだＨ2−Ｎ2ガスを焼成炉に流しながら１５００℃
以上の高温で行われている。However, when these metals are fired in an oxidizing atmosphere, they are oxidized and lose conductivity, so that it is necessary to fire them in a non-oxidizing atmosphere. This firing is 1000
After the debinding process at a temperature of ℃ or more, 1500 ℃ while flowing H2-N2 gas containing water into the firing furnace.
It is performed at the above high temperature.
【０００４】[0004]
【発明が解決しようとする課題】しかし、このような高
温での雰囲気焼成が必要なため、導体を内蔵するセラミ
ックスを製造するには電気代、ガス代などに多額の焼成
費用がかかるという問題があった。また、アルミナセラ
ミックスの表面に導体を形成した場合は、形成したＷや
Ｍｏが酸化する問題から、その上面にメッキを施すなど
の処置が必要となることがあるので、工程がより煩雑と
なっていた。However, since such a high temperature atmosphere firing is required, there is a problem that a large amount of firing cost is required for electricity, gas, etc. to manufacture a ceramic containing a conductor. there were. In addition, when a conductor is formed on the surface of alumina ceramics, the formed W or Mo may be oxidized, so that it may be necessary to perform a treatment such as plating on the upper surface of the conductor, which makes the process more complicated. It was
【０００５】本発明は、上述した従来の導体を内蔵する
アルミナセラミックスが有する課題に鑑みなされたもの
であって、その目的は、大気中で１４００℃以下の温度
で焼成可能な、導体を内蔵するアルミナセラミックスと
その製造方法を提供することにある。The present invention has been made in view of the problems of the above-described conventional alumina ceramics containing a conductor, and its object is to incorporate a conductor that can be fired at a temperature of 1400 ° C. or less in the atmosphere. It is to provide an alumina ceramics and a manufacturing method thereof.
【０００６】[0006]
【課題を解決するための手段】本発明者等は、上記目的
を達成するため、導体として大気中で焼成できるＰｄを
用い、アルミナ原料として高純度で微粒子の原料を用い
て製造すれば、大気中で１４００℃以下の温度で焼成で
きる導体を内蔵したアルミナセラミックスが得られると
の知見を得て本発明を完成した。In order to achieve the above-mentioned object, the present inventors have found that if Pd which can be fired in the atmosphere is used as a conductor and a fine particle material of high purity is used as an alumina material, The present invention has been completed based on the finding that an alumina ceramic containing a conductor that can be fired at a temperature of 1400 ° C. or lower can be obtained.
【０００７】導体にＰｄを用いるのは、１４００℃以上
の融点を持ち、しかも大気中で焼成しても酸化されない
ためである。Ｐｔも使用可能であるが、極めて高価なた
め、コスト的に合わないので好ましくない。また、Ｎｉ
は１４００℃以上の融点を持ち、しかも安価な材料であ
るが、雰囲気焼成が必要となるのでこれも好ましくな
い。Pd is used for the conductor because it has a melting point of 1400 ° C. or higher and is not oxidized even if fired in the atmosphere. Pt can also be used, but it is not preferable because it is extremely expensive and does not match the cost. In addition, Ni
Has a melting point of 1400 ° C. or higher and is an inexpensive material, but this is also not preferable because it requires firing in an atmosphere.
【０００８】上記導体の成分としては、Ｐｄ単体、又は
４０ｗｔ％以下のＡｇを含むＰｄとした（請求項１）。
ＰｄがＡｇを４０ｗｔ％未満含むとき１２８０℃以上の
温度で焼成可能なので、本発明のアルミナ原料を用いれ
ば十分緻密化する。Ｐｄの一部を安価なこのＡｇを置き
替えることによってコストを引き下げることができる。The component of the conductor is Pd alone or Pd containing 40 wt% or less of Ag (claim 1).
When Pd contains less than 40 wt% of Ag, it can be fired at a temperature of 1280 ° C. or higher, so that the alumina raw material of the present invention is used to sufficiently densify it. The cost can be reduced by replacing a part of Pd with this inexpensive Ag.
【０００９】上記製造に用いるアルミナ原料としては、
純度で９９．９％以上のＡｌ2Ｏ3分を有し、平均粒径で
１．０μｍ以下の細かさを有する原料とした（請求項
２）。この原料を用いれば、大気中で１４００℃以下の
温度で焼成しても十分緻密化したセラミックスが得られ
る。純度が９９．９％より低いと１４００℃以下でも焼
結するが粒成長が著しく、緻密化が不十分となる。一方
粒度が平均粒径で１．０μｍより粗いと焼結温度が高く
なり、１４００℃以下の温度では緻密化が不十分とな
る。As the alumina raw material used in the above production,
A raw material having a purity of 99.9% or more of Al 2 O 3 and a fineness of 1.0 μm or less in average particle diameter was used. If this raw material is used, a sufficiently densified ceramic can be obtained even if it is fired at a temperature of 1400 ° C. or lower in the atmosphere. If the purity is lower than 99.9%, sintering will occur even at 1400 ° C or lower, but grain growth will be remarkable and densification will be insufficient. On the other hand, if the average particle size is coarser than 1.0 μm, the sintering temperature becomes high, and at a temperature of 1400 ° C. or lower, the densification becomes insufficient.
【００１０】本発明のアルミナセラミックスの製造方法
をさらに詳細に述べると、純度がＡｌ2Ｏ3で９９．９％
以上で、かつ平均粒径で１．０μｍ以下のアルミナ原料
にバインダーなどの有機添加剤を配合して慣用の方法で
混合し、混合したスラリーをドクターブレード法、押出
し法などでシート状に成形するか、あるいはスラリーを
乾燥してその乾燥した粉末をＣＩＰ法で成形した後、シ
ート状に加工するかなどして所望の厚さのシート状の成
形体を得る。この成形体の表面に前述のＰｄを主成分と
する導体ペーストをスクリーン印刷などで塗布した後、
その成形体を慣用の方法で積層し、積層した積層体を慣
用の方法で焼成して製造することができる。The method for producing the alumina ceramics of the present invention will be described in more detail. The purity of Al 2 O 3 is 99.9%.
The alumina raw material having an average particle size of 1.0 μm or less is blended with an organic additive such as a binder and mixed by a conventional method, and the mixed slurry is formed into a sheet by a doctor blade method, an extrusion method, or the like. Alternatively, the slurry is dried, the dried powder is molded by the CIP method, and then processed into a sheet to obtain a sheet-shaped molded body having a desired thickness. After applying the above-mentioned conductor paste containing Pd as a main component to the surface of this molded body by screen printing or the like,
The molded body can be laminated by a conventional method, and the laminated laminate can be manufactured by firing by a conventional method.
【００１１】以上、導体としてＰｄを主成分とした金属
を用い、アルミナ原料として高純度で微粒子の原料を用
いて大気中で１４００℃以下の温度で焼成することによ
り、導体を内蔵する緻密なアルミナセラミックスが得ら
れる。As described above, a dense alumina containing a conductor is obtained by using a metal containing Pd as a main component as a conductor and using a high-purity fine particle raw material as an alumina raw material in the atmosphere at a temperature of 1400 ° C. or lower. Ceramics are obtained.
【００１２】[0012]
【実施例】以下、本発明の実施例を比較例と共に挙げ、
本発明をより詳細に説明する。EXAMPLES Examples of the present invention will be given below together with comparative examples.
The present invention will be described in more detail.
【００１３】（実施例１〜３） （１）アルミナ原料 Ａｌ2Ｏ3の純度が９９．９９％以上のの大明化学工業
（株）製のＴＭ−ＤＡＲとＡｌ2Ｏ3の純度が９９．９９
％以上のの住友化学工業（株）製のＡＫＰ−３０００を
用いた。その平均粒径を表１に示す。Examples 1 to 3 (1) Alumina Raw Material TM-DAR manufactured by Daimei Chemical Industry Co., Ltd. with Al 2 O 3 purity of 99.99% or more and Al 2 O 3 purity of 99. 99
% Or more of AKP-3000 manufactured by Sumitomo Chemical Co., Ltd. was used. The average particle size is shown in Table 1.
【００１４】（２）シートの成形 アルミナ原料に分散剤、バインダー、溶剤などを加え、
ボールミルで２４時間混合した。このスラリーをドクタ
ーブレード法によって厚みが約２００μｍのシートを成
形した。(2) Forming of sheet A dispersant, a binder, a solvent, etc. are added to an alumina raw material,
Mix for 24 hours on a ball mill. A sheet having a thickness of about 200 μm was formed from this slurry by the doctor blade method.
【００１５】（３）導体ペーストの調製 Ｐｄ粉末として、住友金属鉱山（株）製のＳＦＰ−５０
１Ｐを用い、Ａｇ粉末として、昭栄化学（株）製のＡｇ
−１０２を用い、これらを表１に示す割合で配合した。
これにエチルセルローズをテルピネオールに溶解したも
のを加え、三本ロールミルで混練して導体ペーストを調
製した。(3) Preparation of Conductor Paste As Pd powder, SFP-50 manufactured by Sumitomo Metal Mining Co., Ltd.
1P using Ag powder manufactured by Shoei Chemical Co., Ltd.
-102 was used and these were blended in the proportions shown in Table 1.
A solution prepared by dissolving ethyl cellulose in terpineol was added to this and kneaded with a three-roll mill to prepare a conductor paste.
【００１６】（４）積層体の作製 アルミナシートの表面に調製した導体ペーストをスクリ
ーン印刷し、この印刷したシートを含め必要枚数のシー
トを積み重ね熱圧着して積層体を作製した。(4) Preparation of Laminated Body A prepared conductor paste was screen-printed on the surface of an alumina sheet, and a necessary number of sheets including the printed sheet were stacked and thermocompression bonded to produce a laminated body.
【００１７】（５）アルミナセラミックスの作製 作製した積層体を、大気中で４００℃の温度で脱バイン
ダーした後、大気中で表１に示す温度で焼成してアルミ
ナセラミックスを作製した。(5) Production of Alumina Ceramics The produced laminated body was debindered in the air at a temperature of 400 ° C. and then fired in the air at the temperatures shown in Table 1 to produce alumina ceramics.
【００１８】（６）評価 得られたアルミナセラミックスの導体を含まない部分を
切り出し、それをアルキメデス法で嵩密度を測定し、併
せてセラミックスの表面を研磨して１０倍の顕微鏡で観
察した。その中で、嵩密度が高く、かつポアが観察され
ないもの、即ちセラミックスが充分緻密化されているも
のを良とし、嵩密度が低く、かつポアが観察されるよう
な異状なもの、即ち緻密化していないものを不良とし
た。さらに内部の導体を顕微鏡で観察して導体の剥離な
どの異状が見られたものを不良とした。それらの結果を
表１に示す。(6) Evaluation A conductor-free portion of the obtained alumina ceramics was cut out, and the bulk density was measured by the Archimedes method, and the surface of the ceramics was polished and observed with a 10 × microscope. Among them, those having a high bulk density and in which pores are not observed, that is, those in which the ceramics are sufficiently densified are considered good, and those having a low bulk density and in which pores are observed, that is, densification The ones that have not been made bad. Further, when the conductor inside was observed under a microscope, abnormalities such as peeling of the conductor were found to be defective. The results are shown in Table 1.
【００１９】（比較例１〜２）比較のために、アルミナ
原料として、昭和電工（株）製のＡＬ−１６０ＳＧと住
友化学工業（株）製のＡＬ−Ｍ４１を用い、そのＡｌ2
Ｏ3の純度と平均粒度を表１の如く本発明の範囲外にし
てそのほかは実施例と同様にアルミナセラミックスを作
製し、実施例と同じ方法で評価した。それらの結果を表
１に示す。Comparative Examples 1 and 2 For comparison, AL-160SG manufactured by Showa Denko KK and AL-M41 manufactured by Sumitomo Chemical Co., Ltd. were used as alumina raw materials, and Al 2
Alumina ceramics were produced in the same manner as in the other examples except that the purity and average particle size of O 3 were out of the range of the present invention as shown in Table 1 and evaluated in the same manner as the examples. The results are shown in Table 1.
【００２０】[0020]
【表１】 [Table 1]
【００２１】表１から明らかなように、実施例１〜３に
おいては、嵩密度が３．９ｇ／ｃｍ3前後と極めて高密
度であり、その表面もポアがほとんど認められなかっ
た。また焼結体の内部の導体も異状なく良好なものが得
られた。As is clear from Table 1, in Examples 1 to 3, the bulk density was extremely high at around 3.9 g / cm 3 , and almost no pores were observed on the surface thereof. In addition, the conductor inside the sintered body was also good and good.
【００２２】これに対して本発明の範囲外、即ち、Ａｌ
2Ｏ3の純度が本発明の範囲外にある比較例１において
は、内部の導体については異状はみられないが、嵩密度
が大きく低下しており、その表面のポアも多く認められ
緻密化していなかった。また平均粒径で本発明の範囲外
にある比較例２においても、比較例１と同様であった。On the other hand, outside the scope of the present invention, namely, Al
In Comparative Example 1 in which the purity of 2 O 3 is out of the range of the present invention, no abnormalities are observed in the conductor inside, but the bulk density is greatly reduced, and many pores on the surface are recognized and densified. Didn't. Also in Comparative Example 2 in which the average particle size is outside the range of the present invention, it was the same as Comparative Example 1.
【００２３】[0023]
【発明の効果】以上の通り、本発明にかかる製造方法を
採用すれば、導体を内蔵したアルミナセラミックスを、
大気中で１４００℃以下の温度で焼成することができる
ので、安価で容易に作製できるようになった。また、導
体がセラミックス表面に形成されても耐酸化性に優れて
いるＰｄを用いているので、信頼性の高いセラミックス
製の電気部品が得られるようになった。このことによ
り、ＩＣ基板やヒータ、静電チャックなど様々な分野に
本発明の製品を提供可能となる。As described above, when the manufacturing method according to the present invention is adopted, the alumina ceramics containing the conductor is
Since it can be fired at a temperature of 1400 ° C. or lower in the atmosphere, it can be easily manufactured at low cost. Further, since Pd, which is excellent in oxidation resistance even when the conductor is formed on the surface of the ceramic, is used, it has become possible to obtain a highly reliable ceramic electric component. As a result, the product of the present invention can be provided in various fields such as IC substrates, heaters, and electrostatic chucks.
Claims (2)
おいて、該導体がＰｄ単体、又は４０ｗｔ％以下のＡｇ
を含むＰｄであることを特徴とするアルミナセラミック
ス。1. An alumina ceramic containing a conductor, wherein the conductor is Pd alone or 40 wt% or less of Ag.
Alumina ceramics which is Pd containing.
し、平均粒径で１．０μｍ以下の細かさを有するアルミ
ナ原料を混合して成形し、その成形体にＰｄ単体、又は
４０ｗｔ％以下のＡｇを含むＰｄからなる導体を塗布し
た後、その成形体を積層し、積層した積層体を大気中で
１４００℃以下の温度で焼成することを特徴とするアル
ミナセラミックスの製造方法。2. An alumina raw material having a purity of 99.9% or more of Al 2 O 3 content and an average particle size of 1.0 μm or less is mixed and molded, and the molded body is made of Pd simple substance. Alternatively, a conductor made of Pd containing 40 wt% or less of Ag is applied, the molded bodies are laminated, and the laminated body is fired at a temperature of 1400 ° C. or less in the atmosphere. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6274231A JPH08119720A (en) | 1994-10-14 | 1994-10-14 | Alumina ceramic and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6274231A JPH08119720A (en) | 1994-10-14 | 1994-10-14 | Alumina ceramic and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH08119720A true JPH08119720A (en) | 1996-05-14 |
Family
ID=17538844
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6274231A Withdrawn JPH08119720A (en) | 1994-10-14 | 1994-10-14 | Alumina ceramic and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH08119720A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6265816B1 (en) * | 1998-04-30 | 2001-07-24 | Ngk Spark Plug Co., Ltd. | Spark plug, insulator for spark plug and process for fabricating the insulator |
| CN103681432A (en) * | 2012-08-29 | 2014-03-26 | Toto株式会社 | Electrostatic chuck |
| US9252040B2 (en) | 2012-08-29 | 2016-02-02 | Toto Ltd. | Electrostatic chuck |
| US9300229B2 (en) | 2012-09-12 | 2016-03-29 | Toto Ltd. | Electrostatic chuck |
-
1994
- 1994-10-14 JP JP6274231A patent/JPH08119720A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6265816B1 (en) * | 1998-04-30 | 2001-07-24 | Ngk Spark Plug Co., Ltd. | Spark plug, insulator for spark plug and process for fabricating the insulator |
| CN103681432A (en) * | 2012-08-29 | 2014-03-26 | Toto株式会社 | Electrostatic chuck |
| KR101485438B1 (en) * | 2012-08-29 | 2015-01-22 | 토토 가부시키가이샤 | Electrostatic chuck |
| US9252041B2 (en) | 2012-08-29 | 2016-02-02 | Toto Ltd. | Electrostatic chuck |
| US9252040B2 (en) | 2012-08-29 | 2016-02-02 | Toto Ltd. | Electrostatic chuck |
| US9300229B2 (en) | 2012-09-12 | 2016-03-29 | Toto Ltd. | Electrostatic chuck |
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