JP3359489B2 - Conductive ceramics - Google Patents
Conductive ceramicsInfo
- Publication number
- JP3359489B2 JP3359489B2 JP07790796A JP7790796A JP3359489B2 JP 3359489 B2 JP3359489 B2 JP 3359489B2 JP 07790796 A JP07790796 A JP 07790796A JP 7790796 A JP7790796 A JP 7790796A JP 3359489 B2 JP3359489 B2 JP 3359489B2
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- mol
- oxide
- sintered body
- powder
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Description
【０００１】[0001]
【発明の属する技術分野】本発明は、静電気防止部品、
抵抗体用基体、導電材料、接点、ヒーター、ＶＴＲのガ
イドローラ等として用いられる導電性セラミックスに関
する。The present invention relates to an antistatic component,
The present invention relates to a conductive ceramic used as a substrate for a resistor, a conductive material, a contact, a heater, a guide roller of a VTR, and the like.
【０００２】[0002]
【従来の技術】従来より、例えば半導体製造装置におけ
る搬送用アーム、ハンドリング治具、ウェハ把持ピンセ
ット等の静電気を防止するために、導電性セラミックス
を用いることが行われている。2. Description of the Related Art Conventionally, conductive ceramics have been used in order to prevent static electricity in, for example, a transfer arm, a handling jig, and a wafer gripping tweezer in a semiconductor manufacturing apparatus.
【０００３】この導電性セラミックスとしては、例えば
導電性アルミナセラミックスが知られている。これは、
アルミナ粉末に、導電剤としてアルカリ金属、チタン、
その他の酸化物粉末を添加し、乾式あるいは湿式で混合
後、必要に応じて成形助剤を添加して成形し、所望の導
電性を得るために非酸化性雰囲気で焼成したものであっ
た。As the conductive ceramics, for example, conductive alumina ceramics are known. this is,
Alkali metal, titanium,
Other oxide powders were added, mixed by a dry or wet method, molded as necessary by adding a molding aid, and fired in a non-oxidizing atmosphere to obtain a desired conductivity.
【０００４】また、アルミナを主成分とするセラミック
スに、Ｔｉ，Ｚｒ，Ｈｆ，Ｎｂ等の金属の炭化物又は窒
化物を導電剤として添加したものもある。There is also a ceramic in which a carbide or nitride of a metal such as Ti, Zr, Hf, or Nb is added as a conductive agent to a ceramic containing alumina as a main component.
【０００５】[0005]
【発明が解決しようとする課題】ところが、これらの導
電性アルミナセラミックスは、緻密な焼結体を得るため
にホットプレス（ＨＰ）または熱間静水圧プレス（ＨＩ
Ｐ）により製造する必要があり、生産性が悪いという問
題があった。また、上記導電剤を成すアルカリ金属やチ
タンは還元させないと導電性を有しないことから、非酸
化性雰囲気で焼成しなければならず、製造コストが高く
なるという問題があった。However, these conductive alumina ceramics are hot pressed (HP) or hot isostatically pressed (HI) in order to obtain a dense sintered body.
P), and there is a problem that productivity is poor. In addition, since the alkali metal or titanium constituting the above-mentioned conductive agent does not have conductivity unless it is reduced, it has to be fired in a non-oxidizing atmosphere, resulting in an increase in manufacturing cost.
【０００６】さらに、Ｔｉ，Ｚｒ，Ｈｆ，Ｎｂ等の金属
の炭化物又は窒化物を導電剤として用いたものでは原料
自体が高価であるという問題もあった。Further, there is a problem that raw materials themselves are expensive in the case of using a carbide or nitride of a metal such as Ti, Zr, Hf, Nb or the like as a conductive agent.
【０００７】そこで、本発明は、大気中で緻密に焼結さ
せることができ、製造の容易な導電性セラミックスを得
ることを目的とする。Therefore, an object of the present invention is to obtain a conductive ceramic which can be densely sintered in the air and is easily manufactured.
【０００８】[0008]
【課題を解決するための手段】本発明は、鉄族金属酸化
物の少なくとも一種を１５〜３２モル％と、周期律表第
５ａ族元素酸化物の少なくとも一種を１〜４モル％と、
二酸化マンガン１７〜４７モル％と、アルミナ１７〜７
０モル％からなることを特徴とする。According to the present invention, at least one kind of iron group metal oxide is 15 to 32 mol%, and at least one kind of group 5a element oxide of the periodic table is 1 to 4 mol%.
Manganese dioxide 17-47 mol% and alumina 17-7
0 mol%.
【０００９】ここで、上記鉄族金属の酸化物は、所望の
体積固有抵抗を有する緻密な焼結体を得るために必要な
成分であり、その含有量が１０モル％よりも少ないと体
積固有抵抗が１×１０8 Ω・ｃｍよりも大きくなって絶
縁体に近づき、一方３５モル％よりも多いと焼結時のシ
ミ出しが発生して緻密な焼結体が得られなくなる。した
がって、鉄族金属酸化物の含有量は１０〜３５モル％の
範囲が良く、特に１５〜３２モル％の範囲が好ましい。
なお、鉄族金属としては鉄（Ｆｅ）、コバルト（Ｃ
ｏ）、ニッケル（Ｎｉ）があり、本発明では鉄が好まし
い。Here, the iron group metal oxide is a component necessary for obtaining a dense sintered body having a desired volume specific resistance. If the content is less than 10 mol%, the volume specific volume is reduced. If the resistance is higher than 1 × 10 8 Ω · cm and approaches the insulator, on the other hand, if it is higher than 35 mol%, spots occur during sintering and a dense sintered body cannot be obtained. Therefore, the content of the iron group metal oxide is preferably in the range of 10 to 35 mol%, and particularly preferably in the range of 15 to 32 mol%.
In addition, iron (Fe), cobalt (C
o) and nickel (Ni), and iron is preferred in the present invention.
【００１０】次に第５ａ族元素酸化物は、焼結性を向上
させるために必要な成分であり、その含有量が１．０モ
ル％よりも少ないと混合原料中で不均一となって、安定
した体積固有抵抗を有する焼結体を得られなくなり、５
モル％を超えると緻密な焼結体が得られなくなる。した
がって、第５ａ族元素酸化物の含有量は１．０〜５モル
％の範囲が良く、特に１．０〜４モル％の範囲が好まし
い。なお、第５ａ族元素酸化物としてはバナジウム
（Ｖ）、ニオブ（Ｎｂ）、タンタル（Ｔａ）があり、本
発明ではニオブが好ましい。Next, the Group 5a element oxide is a component necessary for improving sinterability, and if its content is less than 1.0 mol%, it becomes non-uniform in the mixed raw material. A sintered body having a stable volume resistivity cannot be obtained.
If it exceeds mol%, a dense sintered body cannot be obtained. Therefore, the content of the Group 5a element oxide is preferably in the range of 1.0 to 5 mol%, and particularly preferably in the range of 1.0 to 4 mol%. Note that the Group 5a element oxide includes vanadium (V), niobium (Nb), and tantalum (Ta), and niobium is preferable in the present invention.
【００１１】また、二酸化マンガン（ＭｎＯ2 ）は、焼
結性を向上して比較的低温で焼成可能とし、所望の体積
固有抵抗を得るために必要な成分であり、その含有量が
１４．５モル％未満であると体積固有抵抗が１×１０8
Ω・ｃｍよりも大きくなって絶縁体に近づき、５０モル
％を超えると焼結時のシミ出しが発生して緻密な焼結体
が得られなくなる。したがって、二酸化マンガンの含有
量は１４．５〜５０モル％の範囲が良く、特に１７〜４
７モル％の範囲が好ましい。Further, manganese dioxide (MnO 2 ) is a component necessary for improving sinterability and enabling sintering at a relatively low temperature and obtaining a desired volume resistivity, and its content is 14.5. If it is less than mol%, the volume resistivity is 1 × 10 8
When it is larger than Ω · cm and approaches the insulator, if it exceeds 50 mol%, spots occur during sintering, and a dense sintered body cannot be obtained. Therefore, the content of manganese dioxide is preferably in the range of 14.5 to 50 mol%, particularly 17 to 4 mol%.
A range of 7 mol% is preferred.
【００１２】さらに、アルミナ（Ａｌ2 Ｏ3 ）は、焼結
体の緻密性を向上させるために必要な成分であり、その
含有量が１５モル％よりも少ないと焼結体にクラックが
発生しやすく、７３．８モル％よりも多いと体積固有抵
抗が１×１０8 Ω・ｃｍよりも大きくなって絶縁体に近
づいてしまう。したがって、アルミナの含有量は１５〜
７３．８モル％の範囲が良く、特に１７〜７０モル％の
範囲が好ましい。なお、焼結体の緻密性の点からは、ア
ルミナの含有量を２５〜７３．８モル％の範囲とするこ
とが好ましい。Alumina (Al 2 O 3 ) is a component necessary for improving the compactness of the sintered body. If the content is less than 15 mol%, cracks occur in the sintered body. When the content is more than 73.8 mol%, the volume resistivity becomes larger than 1 × 10 8 Ω · cm, and approaches the insulator. Therefore, the content of alumina is 15 to
The range of 73.8 mol% is good, and the range of 17 to 70 mol% is particularly preferable. In addition, from the viewpoint of the denseness of the sintered body, the content of alumina is preferably in the range of 25 to 73.8 mol%.
【００１３】そして、本発明の導電性セラミックスで
は、酸化鉄１７〜２８モル％、酸化ニオブ１〜３．５モ
ル％、二酸化マンガン２０〜４１モル％、アルミナ２８
〜６７モル％の範囲としたものが最適である。In the conductive ceramic of the present invention, 17 to 28 mol% of iron oxide, 1 to 3.5 mol% of niobium oxide, 20 to 41 mol% of manganese dioxide, and 28% of alumina
Optimally, the content is in the range of ~ 67 mol%.
【００１４】なお、上記成分以外に、原料粉末中や製造
工程で混入する不純物として、シリカ（ＳｉＯ2 ）を
０．１重量％以下、酸化カルシウム（ＣａＯ）を０．０
５重量％以下、酸化クロム（Ｃｒ2 Ｏ3 ）、酸化コバル
ト（ＣｏＯ）、酸化マグネシクム（ＭｇＯ）等を合計
０．１重量％以下の範囲で含んでいても良い。[0014] In addition to the above components, as impurities mixed in the raw material powder or in the production process, silica (SiO 2 ) is 0.1% by weight or less, and calcium oxide (CaO) is
It may contain 5% by weight or less, chromium oxide (Cr 2 O 3 ), cobalt oxide (CoO), magnesium oxide (MgO) or the like in a total range of 0.1% by weight or less.
【００１５】本発明の導電性セラミックスを製造する場
合は、例えば、鉄族金属の酸化物粉末、第５ａ族元素酸
化物粉末、二酸化マンガン粉末、アルミナ粉末を用い、
あるいは焼成中にこれらの材料に変化しうる前記材料の
水酸化物粉末、炭酸化粉末を用い、これらを湿式または
乾式で混合し、湿式の場合はスプレードライ等で造粒し
た後、所望形状に成形して、酸化雰囲気で１２４０〜１
３５０℃にて１〜３時間焼成する。When the conductive ceramic of the present invention is produced, for example, an oxide powder of an iron group metal, an oxide powder of a Group 5a element, a manganese dioxide powder, and an alumina powder are used.
Alternatively, using a hydroxide powder or a carbonated powder of the above-mentioned material which can be changed into these materials during firing, mixing these in a wet or dry method, and in the case of a wet method, granulating by spray drying or the like, and then forming into a desired shape Molded, 1240-1 in oxidizing atmosphere
Bake at 350 ° C for 1 to 3 hours.
【００１６】ここで、焼成温度を１２４０〜１３５０℃
としたのは、１２４０℃未満であると充分に焼結せずに
焼結体の吸水率が０．１％を超えてしまい、さらに体積
固有抵抗が１×１０8 Ω・ｃｍよりも大きくなって絶縁
体に近づき、一方１３５０℃を超えるとオーバーシンタ
ーとなって吸水率が０．１％を超えてしまうためであ
る。Here, the firing temperature is set to 1240 to 1350 ° C.
The reason is that if the temperature is lower than 1240 ° C., the sintered body does not sinter sufficiently, the water absorption of the sintered body exceeds 0.1%, and the volume resistivity becomes larger than 1 × 10 8 Ω · cm. When the temperature exceeds 1350 ° C., oversintering occurs and the water absorption exceeds 0.1%.
【００１７】また、本発明の導電性セラミックスは、大
気中の酸化雰囲気で焼成しても充分な導電性を有し、そ
の体積固有抵抗を１０4 〜１０8 Ω・ｃｍとすることが
できる。ここで、体積固有抵抗を１０4 〜１０8 Ω・ｃ
ｍとしたのは、静電気を除去するとともに、適度な絶縁
性を有するためである。The conductive ceramic of the present invention has sufficient conductivity even when fired in an oxidizing atmosphere in the air, and can have a volume resistivity of 10 4 to 10 8 Ω · cm. Here, the volume resistivity is 10 4 to 10 8 Ω · c.
The reason for m is to remove static electricity and to have an appropriate insulating property.
【００１８】このような本発明の導電性セラミックス
は、半導体製造装置における搬送用アーム、ハンドリン
グ治具、ウェハ把持用ピンセット等に用いれば、静電気
を除去して半導体に悪影響を及ぼすことを防止できる。If the conductive ceramic of the present invention is used for a transfer arm, a handling jig, a wafer gripping tweezer, or the like in a semiconductor manufacturing apparatus, it is possible to prevent static electricity from being adversely affected on the semiconductor.
【００１９】あるいは、磁気ディスクドライブ装置にお
いて複数の磁気ディスク間に挟み込んで位置決めを行う
ためのディスクスペーサとして用いれば、静電気を除去
して磁気ディスクに悪影響を及ぼすことを防止できる。Alternatively, if the magnetic disk drive device is used as a disk spacer for positioning by sandwiching the magnetic disk between a plurality of magnetic disks, static electricity can be removed to prevent the magnetic disks from being adversely affected.
【００２０】さらに、その他の静電気防止部品や、抵抗
体用基板、導電材料、接点、ヒーター、ＶＴＲのガイド
ローラ等に本発明の導電性セラミックスを使用すること
ができる。Further, the conductive ceramics of the present invention can be used for other antistatic parts, resistor substrates, conductive materials, contacts, heaters, VTR guide rollers, and the like.
【００２１】[0021]
【実施例】酸化鉄（Ｆｅ2 Ｏ3 ）粉末、酸化ニオブ（Ｎ
ｂ2 Ｏ5 ）粉末、二酸化マンガン（ＭｎＯ2 ）粉末、ア
ルミナ（Ａｌ2 Ｏ3 ）粉末を用意し、焼結体の組成が表
１に示す割合となるように秤量後、回転ミルにて湿式混
合した。混合後のスラリーをスプレードライにて乾燥
し、焼結用原料とした。これを、プレス成形し、大気中
にて表１に示す温度で２時間焼成し、直径１７ｍｍ、厚
み３ｍｍの円板状の焼結体を得た。DESCRIPTION OF THE PREFERRED EMBODIMENTS Iron oxide (Fe 2 O 3 ) powder, niobium oxide (N
b 2 O 5 ) powder, manganese dioxide (MnO 2 ) powder, and alumina (Al 2 O 3 ) powder were prepared, weighed so that the composition of the sintered body had the ratio shown in Table 1, and then wet weighed with a rotary mill. Mixed. The mixed slurry was dried by spray drying to obtain a raw material for sintering. This was press-formed and fired in the atmosphere at the temperature shown in Table 1 for 2 hours to obtain a disc-shaped sintered body having a diameter of 17 mm and a thickness of 3 mm.
【００２２】この両端面を研摩して試料の厚みを２ｍｍ
とし、その面に電極を塗布して体積固有抵抗を求めた。
同時に焼成した他の焼結体をＪＩＳ Ｃ ２１４１に定
める吸水率の測定方法に基づき吸水率を求めた。これら
の結果を表２に示す。The both end faces are polished to reduce the thickness of the sample to 2 mm.
The surface was coated with an electrode to determine the volume resistivity.
The water absorption of another sintered body fired at the same time was determined based on the method of measuring the water absorption specified in JIS C 2141. Table 2 shows the results.
【００２３】この結果より、酸化鉄（Ｆｅ2Ｏ3）の含有
量が１５モル％未満であると体積固有抵抗値が１×１０
7Ω・ｃｍよりも大きくなり、一方３５モル％を超える
と焼結体からのシミ出しが多くなって緻密な焼結体が得
られなかった。また、酸化ニオブ（Ｎｂ2Ｏ5）の含有量
が１モル％未満では体積固有抵抗値が不安定となり、５
モル％を超えると緻密な焼結体が得られなかった。The results show that when the content of iron oxide (Fe 2 O 3 ) is less than 15 mol%, the volume resistivity value becomes 1 × 10 5
If it exceeds 7 Ω · cm, on the other hand, if it exceeds 35 mol%, stains from the sintered body increase and a dense sintered body cannot be obtained. If the content of niobium oxide (Nb 2 O 5 ) is less than 1 mol%, the volume resistivity becomes unstable and the
If it exceeds mol%, a dense sintered body cannot be obtained.
【００２４】これらに対し、本発明の範囲内のものは、
体積固有抵抗値が４．１×１０5〜７．２×１０6Ω・ｃ
ｍの範囲内で、吸水率が０．０６％以下と緻密に焼結し
ていることが確認された。In contrast, those within the scope of the present invention are:
Volume resistivity value of 4.1 × 10 5 to 7.2 × 10 6 Ω · c
Within the range of m, it was confirmed that the water absorption was 0.06% or less and the sintering was performed densely.
【００２５】[0025]
【表１】 [Table 1]
【００２６】[0026]
【表２】 [Table 2]
【００２７】次に、鉄族金属酸化物として、酸化鉄（Ｆ
ｅ2 Ｏ3 ）粉末だけでなく酸化ニッケル（ＮｉＯ）粉末
や酸化コバルト（ＣｏＯ）粉末も用い、第５ａ族元素酸
化物として酸化ニオブ（Ｎｂ2 Ｏ5 ）粉末だけでなく酸
化タンタル（Ｔａ2 Ｏ5 ）粉末や酸化バナジウム（Ｖ2
Ｏ5 ）粉末も用いて上記と同様の評価を行った。この結
果を表３、４に示す。Next, iron oxide (F
e 2 O 3) alone without using even nickel oxide (NiO) powder and cobalt oxide (CoO) powder powder, niobium oxide as the 5a group element oxide (Nb 2 O 5) tantalum oxide not only powder (Ta 2 O 5 ) Powder or vanadium oxide (V 2
The same evaluation as above was performed using O 5 ) powder. The results are shown in Tables 3 and 4.
【００２８】この結果より、鉄族金属酸化物の含有量が
１５モル％未満であると、体積固有抵抗値が１×１０7
Ω・ｃｍ以上となり、一方３２モル％を越えると焼結体
からのシミ出しが多くなって緻密な焼結体が得られなか
った。また、第５ａ族元素酸化物の含有量が１モル％未
満では体積固有抵抗値が不安定となり、５モル％を超え
ると緻密な焼結体が得られなかった。According to the results, when the content of the iron group metal oxide is less than 15 mol%, the volume resistivity value is 1 × 10 7.
On the other hand, if it exceeds 32 mol%, the amount of stains from the sintered body increases, and a dense sintered body cannot be obtained. When the content of the Group 5a element oxide was less than 1 mol%, the volume resistivity was unstable, and when it exceeded 5 mol%, a dense sintered body could not be obtained.
【００２９】これらに対し、本発明の範囲内のものは、
体積固有抵抗値が１×１０7Ω・ｃｍ未満の範囲内で、
吸水率が０．１％以下と緻密に焼結していることが確認
された。On the other hand, those within the scope of the present invention are:
When the volume resistivity is less than 1 × 10 7 Ω · cm,
It was confirmed that the sintered body was densely sintered with a water absorption of 0.1% or less.
【００３０】[0030]
【表３】 [Table 3]
【００３１】[0031]
【表４】 [Table 4]
【００３２】[0032]
【発明の効果】以上のように本発明によれば、鉄族金属
酸化物の少なくとも一種を１５〜３２モル％と、周期律
表第５ａ族元素酸化物の少なくとも一種を１〜４モル％
と、二酸化マンガン１７〜４７モル％と、アルミナ１７
〜７０モル％から導電性セラミックスを構成することに
よって、吸水率が０．１％以下で、体積固有抵抗値が１
×１０7Ω・ｃｍ未満の導電性セラミックスを大気中の
酸化雰囲気の焼成によって容易に製造することができ
る。As described above, according to the present invention, at least one of the iron group metal oxides is 15 to 32 mol%, and at least one of the group 5a element oxides of the periodic table is 1 to 4 mol%.
And 17 to 47 mol% of manganese dioxide and alumina 17
By constituting the conductive ceramic from 70 to 70 mol%, the water absorption is 0.1% or less and the volume resistivity is 1%.
Conductive ceramics of less than × 10 7 Ω · cm can be easily manufactured by firing in an oxidizing atmosphere in the air.
【００３３】したがって、各種静電気防止部品等に好適
な導電性セラミックスを簡単な製造工程で低コストで製
造することができる。Accordingly, conductive ceramics suitable for various antistatic parts can be manufactured at a low cost by a simple manufacturing process.
Claims (1)
３２モル％と、周期律表第５ａ族元素酸化物の少なくと
も一種を１〜４モル％と、二酸化マンガン１７〜４７モ
ル％と、アルミナ１７〜７０モル％からなることを特徴
とする導電性セラミックス。1. The method according to claim 1, wherein at least one of the iron group metal oxides is 15 to
32 % by mole, 1 to 4 % by mole of at least one of Group 5a element oxides of the periodic table, 17 to 47 % by mole of manganese dioxide, and 17 to 70 % by mole of alumina .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07790796A JP3359489B2 (en) | 1996-03-29 | 1996-03-29 | Conductive ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP07790796A JP3359489B2 (en) | 1996-03-29 | 1996-03-29 | Conductive ceramics |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH09268060A JPH09268060A (en) | 1997-10-14 |
| JP3359489B2 true JP3359489B2 (en) | 2002-12-24 |
Family
ID=13647152
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP07790796A Expired - Fee Related JP3359489B2 (en) | 1996-03-29 | 1996-03-29 | Conductive ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3359489B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5998787B2 (en) | 2011-12-02 | 2016-09-28 | Toto株式会社 | Semiconductive ceramic sintered body |
| JP6056312B2 (en) | 2011-12-02 | 2017-01-11 | Toto株式会社 | Semiconductive ceramic sintered body |
-
1996
- 1996-03-29 JP JP07790796A patent/JP3359489B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH09268060A (en) | 1997-10-14 |
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