JPH07144983A - Alumina dielectric having enhanced electric conductivity of surface and its production - Google Patents
Alumina dielectric having enhanced electric conductivity of surface and its productionInfo
- Publication number
- JPH07144983A JPH07144983A JP5314205A JP31420593A JPH07144983A JP H07144983 A JPH07144983 A JP H07144983A JP 5314205 A JP5314205 A JP 5314205A JP 31420593 A JP31420593 A JP 31420593A JP H07144983 A JPH07144983 A JP H07144983A
- Authority
- JP
- Japan
- Prior art keywords
- alumina dielectric
- dielectric
- alumina
- transition metal
- metal oxide
- 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
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、体積抵抗に比べて表面
誘電性を向上したアルミナ誘電体及びその製造方法に関
し、特に静電チャックやセラミックスコンデンサ−など
の“物質の誘電的性質”を利用する製品の材料に好適な
アルミナ誘電体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 an alumina dielectric having an improved surface dielectric property as compared with volume resistance and a method for manufacturing the same, and in particular, utilizes the "dielectric property of a material" such as an electrostatic chuck or a ceramic capacitor. The present invention relates to an alumina dielectric suitable for a material of a product and a manufacturing method thereof.
【０００２】[0002]
【従来の技術】アルミナセラミックスは、高硬度、高弾
性率を有し、耐薬品性、耐摩耗性、耐熱性に優れ、しか
もセラミックスにしては比較的安価である等の特徴を有
している。そのため、アルミナセラミックスは、例えば
機械部品のようなエンジニアリングセラミックス等とし
て最も普及しているセラミックスである。2. Description of the Related Art Alumina ceramics have characteristics such as high hardness and high elastic modulus, excellent chemical resistance, abrasion resistance, and heat resistance, and relatively inexpensive ceramics. . Therefore, alumina ceramics are the most popular ceramics as engineering ceramics such as machine parts.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、このア
ルミナセラミックスを、例えば静電チャックのような誘
電的性質を利用する製品に適用した場合、該セラミック
スの比誘電率の低さ等の理由により、吸着力が小さく、
かつ応答性が悪いなどの不都合が生じる。However, when this alumina ceramics is applied to a product using dielectric properties such as an electrostatic chuck, it is adsorbed because of the low relative permittivity of the ceramics. Small force,
In addition, inconvenience such as poor response occurs.
【０００４】ところで、静電チャックに応用する場合の
吸着力の低さを改善する方法として、ジョンソンラ−ベ
ック力の利用が考えられる。これは、チャック本体と被
吸着物との間に微小な電流を流すことにより発現する力
を利用するものであり、これによりその界面に蓄積する
体積電荷が静電力を向上させるものと考えられる。By the way, the use of the Johnson-Rahbek force can be considered as a method for improving the low attraction force when applied to an electrostatic chuck. This utilizes the force developed by passing a minute current between the chuck body and the object to be attracted, and it is considered that the volume charge accumulated at the interface improves the electrostatic force.
【０００５】このジヨンソンラ−ベック力を利用するに
当っては、チャックの表面のみを導電性にすれば良く、
チャック内部の体積抵抗まで下げるのは、漏れ電流の不
必要な増加などの事態を招き、不利である。In utilizing this Jonson-Rahbek force, it suffices to make only the surface of the chuck conductive.
Reducing the volume resistance inside the chuck is disadvantageous because it causes an unnecessary increase in leakage current.
【０００６】そこで、本発明は、表面のみを導電性にす
ることを意図したものであって、アルミナセラミックス
を、例えば静電チャックのような誘電的性質を利用する
製品に適用することを技術的課題とし、そのため、該セ
ラミックスの有する前記した吸着力の低さ、応答性の悪
さ等の不都合を解消し、体積抵抗に比べて表面導電性を
向上したアルミナ誘電体を提供することを目的とする。Therefore, the present invention is intended to make only the surface conductive, and it is technically applicable to apply the alumina ceramics to a product utilizing dielectric properties such as an electrostatic chuck. Therefore, it is an object of the present invention to solve the above-mentioned inconveniences such as low adsorption force and poor response of the ceramics, and to provide an alumina dielectric having improved surface conductivity as compared with volume resistance. .
【０００７】[0007]
【課題を解決するための手段】本発明は、微量の遷移金
属成分を添加したアルミナ誘電体の表面に導電成分を形
成することを特徴とし、これにより前記目的とする“体
積抵抗に比べて表面導電性を向上したアルミナ誘電体”
を提供するものである。The present invention is characterized in that a conductive component is formed on the surface of an alumina dielectric to which a trace amount of a transition metal component is added, whereby the target "surface resistance as compared with the volume resistance" is obtained. Alumina dielectric with improved conductivity ”
Is provided.
【０００８】即ち、本発明のアルミナ誘電体は、「遷移
金属酸化物を添加してなるアルミナ誘電体の表面部に存
在する酸素成分の低次化により表面部に一部導電成分を
形成してなることを特徴とする体積抵抗に比べて表面導
電性を向上したアルミナ誘電体。」を要旨とする。That is, in the alumina dielectric of the present invention, "a conductive component is partially formed on the surface by lowering the oxygen component existing on the surface of the alumina dielectric obtained by adding the transition metal oxide. Alumina dielectric with improved surface conductivity compared to volume resistance. ”
【０００９】また、本発明のアルミナ誘電体の製造方法
は、「遷移金属酸化物を添加してなるアルミナ誘電体
を、還元性ガス雰囲気中、1000〜1400℃で熱処理し、表
面部に存在する酸素成分の低次化により表面部に一部導
電成分を形成することを特徴とする表面導電性を向上し
たアルミナ誘電体の製造方法。」を要旨とする。In addition, the method for producing an alumina dielectric of the present invention is that "alumina dielectric prepared by adding a transition metal oxide is heat-treated at 1000 to 1400 ° C. in a reducing gas atmosphere to be present on the surface portion. A method for producing an alumina dielectric having improved surface conductivity, which is characterized in that a conductive component is partially formed on the surface portion by lowering the oxygen component. "
【００１０】以下、本発明を詳細に説明する。本発明
は、アルミナ誘電体の表面に誘電性を付与するため、表
面型半導体コンデンサ−を作製する手段を利用して、微
量の遷移金属成分を添加し、焼結したアルミナ誘電体を
還元性ガス雰囲気中で熱処理し、酸素の低次化を図るこ
とによって表面に一部導電成分を形成させるものであ
る。The present invention will be described in detail below. In order to impart dielectric properties to the surface of the alumina dielectric, the present invention utilizes a means for producing a surface-type semiconductor capacitor to add a trace amount of a transition metal component and to sinter the sintered alumina dielectric with a reducing gas. A heat treatment is performed in an atmosphere to lower the order of oxygen, so that a conductive component is partially formed on the surface.
【００１１】上記遷移金属酸化物としては、TiO2、SnO2
等の単純な酸化物を使用することができるが、より誘電
率向上が期待できる複合酸化物、例えばCaTiO3、SrTiO3
等のペロブスカイト型チタン酸塩を用いるのが好まし
い。また、本発明において、他の物性を改善するために
Y2O3、Nd2O3等の稀土類金属酸化物やSiO2などを添加す
ることもでき、これも本発明に包含されるものである。The above transition metal oxides include TiO 2 and SnO 2
Although simple oxides such as Al can be used, composite oxides that can be expected to improve the dielectric constant, such as CaTiO 3 and SrTiO 3
It is preferable to use perovskite type titanates such as In addition, in order to improve other physical properties in the present invention,
Rare earth metal oxides such as Y 2 O 3 and Nd 2 O 3 and SiO 2 can be added, and these are also included in the present invention.
【００１２】熱処理時に供給する還元性ガスとしては、
N2／H2混合ガス、N2ガスをイソプロピルアルコ−ル中で
バブリングしたもの等何れも使用することができるが、
H2ガス単味のようにあまり還元性の強いものでは、誘電
体内部まで導電性になるため好ましくない。そのため、
N2／H2混合ガスの例で言えば、H2濃度は多くても10％以
下とするのが好ましい。The reducing gas supplied during the heat treatment is
Any of N 2 / H 2 mixed gas, bubbling N 2 gas in isopropyl alcohol, etc. can be used,
A substance having a very strong reducing property such as H 2 gas alone is not preferable because the inside of the dielectric becomes conductive. for that reason,
In the case of the N 2 / H 2 mixed gas, the H 2 concentration is preferably 10% or less at most.
【００１３】本発明によるアルミナ誘電体の導電性は、
熱処理時の温度、時間、還元性ガスの種類、及びガス流
量等の因子によって制御される。このうち熱処理時の温
度については、1000℃未満では、酸素の低次化効果が不
十分なため好ましくなく、また1400℃以上では、アルミ
ナの粒成長による物性低下が考えられるので好ましくな
い。The conductivity of the alumina dielectric according to the present invention is
It is controlled by factors such as temperature, time during heat treatment, type of reducing gas, and gas flow rate. Of these, if the temperature during the heat treatment is less than 1000 ° C., the oxygen lowering effect is insufficient, and if it is 1400 ° C. or more, the physical properties are likely to deteriorate due to grain growth of alumina, which is not preferable.
【００１４】[0014]
【実施例】次に、本発明の実施例を挙げ、本発明を具体
的に説明する。EXAMPLES Next, the present invention will be specifically described with reference to examples of the present invention.
【００１５】（実施例）アルミナ原料として、大明化学
工業社製のタイミクロンTM-DAR(平均粒径：0.1μｍ、純
度：99.99％)を用い、これに表１に示す配合割合で微量
成分を添加し、アルミナ磁器性ボ−ルミルで３時間乾式
混合した。これを、１軸加圧プレスによって20φ×5ｔ
のペレットに成形し、電気炉で1300℃、２時間焼結して
サンプルとした。なお、本実施例において、SiO2を微量
添加するが(表１参照)、これは機械的強度を増進するた
めであり、本発明を構成する必須成分ではない。(Example) As the alumina raw material, Taimicron TM-DAR (average particle size: 0.1 μm, purity: 99.99%) manufactured by Daimei Chemical Industry Co., Ltd. was used, and a trace amount of components was added in the mixing ratio shown in Table 1. Add and dry mix for 3 hours with an alumina porcelain ball mill. 20φ × 5t by uniaxial press
Was molded into pellets and sintered in an electric furnace at 1300 ° C. for 2 hours to obtain a sample. In this example, a small amount of SiO 2 is added (see Table 1), but this is to enhance the mechanical strength and is not an essential component of the present invention.
【００１６】[0016]
【表１】 [Table 1]
【００１７】得られた焼結サンプルについて、表２に示
す還元性ガス及び熱処理条件で熱処理を行った。この熱
処理後のサンプル表面にガ−ドリング(内径：9φ、外
径：13φ)を用いてド−タイトを塗布し、中心電極と保
護電極をつけ、裏面にド−タイトをベタ塗りして抵抗測
定用サンプルとした。The resulting sintered sample was heat-treated under the reducing gas and heat-treatment conditions shown in Table 2. After this heat treatment, apply the dotite to the surface of the sample using a guard ring (inner diameter: 9φ, outer diameter: 13φ), attach the center electrode and the protective electrode, and apply the dotite solidly to the back surface to measure the resistance. Was used as a sample.
【００１８】測定には絶縁抵抗計を用い、直流電圧50V
を印加して１分後に中心電極と裏面電極間の値(Ｒｖ)及
び中心電極と保護電極間の値(Ｒｓ)を読み取り、次式
(1)及び(2)に従って体積抵抗と表面抵抗を算出した。そ
の結果を表２に示す。An insulation resistance tester was used for the measurement, and the DC voltage was 50V.
One minute after applying the voltage, the value (Rv) between the center electrode and the back electrode and the value (Rs) between the center electrode and the protective electrode are read and
The volume resistance and surface resistance were calculated according to (1) and (2). The results are shown in Table 2.
【００１９】・式(1)……体積抵抗＝Ｒｖ・(πｄ2)／４
ｔ ・式(2)……表面抵抗＝Ｒｓ・π(Ｄ＋ｄ)／(Ｄ−ｄ) ［式(1)及び式(2)中、ｄは中心電極の径(9φ)、Ｄは保
護電極の内径(13φ)、ｔはサンプルの厚さである。］Formula (1) ... Volume resistance = Rv. (Πd 2 ) / 4
t ・ Equation (2) …… Surface resistance = Rs ・ π (D + d) / (D−d) [In the equations (1) and (2), d is the diameter of the center electrode (9φ), and D is the protective electrode. Inner diameter (13φ), t is the thickness of the sample. ]
【００２０】（比較例）なお、比較のため、前記実施例
における“還元性ガス中での熱処理”を行わない未処理
のアルミナ焼結サンプルについて、実施例と同様に体積
抵抗及び表面抵抗を算出した。その結果を表２に併記し
た。(Comparative Example) For comparison, the volume resistance and surface resistance of the untreated alumina sintered sample which was not subjected to the "heat treatment in a reducing gas" in the above-mentioned Example were calculated in the same manner as in the Example. did. The results are also shown in Table 2.
【００２１】[0021]
【表２】 [Table 2]
【００２２】表２から、未処理品(比較例)に比べて、還
元性ガス中で熱処理したサンプル(実施例)では、表面抵
抗、体積抵抗のいずれも低下しており、より導電性にな
っていることが伺われ、しかも、その表面抵抗、体積抵
抗の低下程度にかなり差が認められた。即ち、本発明の
実施例であるサンプルでは、このサンプル内部での導電
性は、その体積抵抗の低下割合から見て未処理品(比較
例)の105倍ぐらいに留まっているのに対し、表面の導電
性は、その表面抵抗の低下割合から約1013倍に向上して
いることが認められた。From Table 2, as compared with the untreated product (Comparative Example), the sample (Example) heat-treated in a reducing gas had lower surface resistance and volume resistance, and became more conductive. However, there was a considerable difference in the degree of reduction in surface resistance and volume resistance. That is, in the sample which is an example of the present invention, the conductivity inside the sample is about 10 5 times that of the untreated product (comparative example) in view of the reduction rate of its volume resistance. It was confirmed that the conductivity of the surface was improved about 10 13 times from the reduction rate of the surface resistance.
【００２３】[0023]
【発明の効果】本発明は、以上詳記したとおり、遷移金
属酸化物を添加してなるアルミナ誘電体を還元性ガス雰
囲気中で熱処理し、アルミナ誘電体の表面に導電成分を
形成することを特徴とし、これにより体積抵抗に比べて
表面導電性を向上したアルミナ誘電体を得ることができ
る効果が生じる。そして、本発明により、静電チャック
のみならず、トリマ−抵抗、ＣＲ複合材料、ハイブリッ
ドＩＣ基板などへの応用が期待できる誘電材料を提供す
ることができる。As described in detail above, according to the present invention, an alumina dielectric formed by adding a transition metal oxide is heat-treated in a reducing gas atmosphere to form a conductive component on the surface of the alumina dielectric. Characteristically, this brings about an effect that an alumina dielectric having improved surface conductivity as compared with volume resistance can be obtained. Further, according to the present invention, it is possible to provide a dielectric material which is expected to be applied to not only an electrostatic chuck but also a trimmer resistor, a CR composite material, a hybrid IC substrate, and the like.
Claims (4)
誘電体の表面部に存在する酸素成分の低次化により表面
部に導電成分を形成してなることを特徴とする体積抵抗
に比べて表面導電性を向上したアルミナ誘電体。1. Compared with volume resistance, which is characterized in that a conductive component is formed on the surface portion by lowering the oxygen component existing on the surface portion of the alumina dielectric material to which a transition metal oxide is added. Alumina dielectric with improved surface conductivity.
誘電体を、還元性ガス雰囲気中、1000〜1400℃で熱処理
し、表面部に存在する酸素成分の低次化により表面部に
導電成分を形成することを特徴とする表面導電性を向上
したアルミナ誘電体の製造方法。2. An alumina dielectric containing a transition metal oxide added thereto is heat-treated at 1000 to 1400 ° C. in a reducing gas atmosphere to lower the oxygen component existing on the surface to reduce the conductive component on the surface. A method for producing an alumina dielectric having improved surface conductivity, comprising:
等の酸化物、又は、CaTiO3、SrTiO3等のペロブスカイト
型チタン酸塩を用いることを特徴とする請求項２記載の
表面導電性を向上したアルミナ誘電体の製造方法。3. The transition metal oxide includes TiO 2 and SnO 2
The method for producing an alumina dielectric with improved surface conductivity according to claim 2, characterized in that an oxide such as or the like or a perovskite type titanate such as CaTiO 3 or SrTiO 3 is used.
ス、又は、N2ガスをイソプロピルアルコ−ル中でバブリ
ングして得られるN2ガスを用いることを特徴とする請求
項２記載の表面導電性を向上したアルミナ誘電体の製造
方法。As claimed in claim 4, wherein the reducing gas, N 2 / H 2 mixed gas, or isopropyl N 2 gas alcohol - according to claim 2, wherein the use of N 2 gas obtained by bubbling in Le Of manufacturing an alumina dielectric having improved surface conductivity of a.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5314205A JPH07144983A (en) | 1993-11-19 | 1993-11-19 | Alumina dielectric having enhanced electric conductivity of surface and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5314205A JPH07144983A (en) | 1993-11-19 | 1993-11-19 | Alumina dielectric having enhanced electric conductivity of surface and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH07144983A true JPH07144983A (en) | 1995-06-06 |
Family
ID=18050544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5314205A Pending JPH07144983A (en) | 1993-11-19 | 1993-11-19 | Alumina dielectric having enhanced electric conductivity of surface and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07144983A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002226269A (en) * | 2001-01-30 | 2002-08-14 | Wicera Co Ltd | Conductive ceramic and its manufacturing method |
| WO2012091062A1 (en) * | 2010-12-28 | 2012-07-05 | 京セラ株式会社 | Ceramic structure with insulating layer, ceramic structure with metal layer, charged particle beam emitter, and method of the manufacturing ceramic structure with insulating layer |
| JP2015529616A (en) * | 2012-07-09 | 2015-10-08 | コーニンクレッカ フィリップス エヌ ヴェ | Method for treating a surface layer of an apparatus composed of alumina, and apparatus corresponding to the method, in particular parts of an X-ray tube |
-
1993
- 1993-11-19 JP JP5314205A patent/JPH07144983A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002226269A (en) * | 2001-01-30 | 2002-08-14 | Wicera Co Ltd | Conductive ceramic and its manufacturing method |
| WO2012091062A1 (en) * | 2010-12-28 | 2012-07-05 | 京セラ株式会社 | Ceramic structure with insulating layer, ceramic structure with metal layer, charged particle beam emitter, and method of the manufacturing ceramic structure with insulating layer |
| JP5787902B2 (en) * | 2010-12-28 | 2015-09-30 | 京セラ株式会社 | Ceramic structure with insulating layer, ceramic structure with metal body, charged particle beam emitting device, and method of manufacturing ceramic structure with insulating layer |
| JP2015529616A (en) * | 2012-07-09 | 2015-10-08 | コーニンクレッカ フィリップス エヌ ヴェ | Method for treating a surface layer of an apparatus composed of alumina, and apparatus corresponding to the method, in particular parts of an X-ray tube |
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