JPH0725620A - Production of ruthenium dioxide fine powder - Google Patents
Production of ruthenium dioxide fine powderInfo
- Publication number
- JPH0725620A JPH0725620A JP19187693A JP19187693A JPH0725620A JP H0725620 A JPH0725620 A JP H0725620A JP 19187693 A JP19187693 A JP 19187693A JP 19187693 A JP19187693 A JP 19187693A JP H0725620 A JPH0725620 A JP H0725620A
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- ruthenium dioxide
- dioxide fine
- production
- acid
- 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
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、厚膜抵抗体の導電物と
して有用である二酸化ルテニウム微粉末の製造方法に関
するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing fine ruthenium dioxide powder which is useful as a conductor of a thick film resistor.
【０００２】[0002]
【従来の技術】空気中等酸化雰囲気で焼成される厚膜抵
抗体用の抵抗ペーストには、導電物として二酸化ルテニ
ウム微粉末やルテニウム酸鉛微粉末が用いられている。
一般に、二酸化ルテニウムは低抵抗値から高抵抗値まで
広い範囲の導電物として用いられ、ルテニウム酸鉛は高
抵抗値用の導電物として用いられている。ところで、二
酸化ルテニウムを得る従来方法としては、塩化ルテニウ
ムをアルカリで中和して得た沈殿を熱処理する方法や、
金属ルテニウムをアルカリ溶解または溶融してできるル
テニウム酸アルカリ塩の水溶液に有機物または酸を加え
て得た沈殿を熱処理する方法がある。2. Description of the Related Art A ruthenium dioxide fine powder or a lead ruthenate fine powder is used as a conductive material in a resistance paste for a thick film resistor that is fired in an oxidizing atmosphere such as air.
Generally, ruthenium dioxide is used as a conductor in a wide range from low resistance to high resistance, and lead ruthenate is used as a conductor for high resistance. By the way, as a conventional method for obtaining ruthenium dioxide, a method of heat treating a precipitate obtained by neutralizing ruthenium chloride with an alkali,
There is a method of heat-treating a precipitate obtained by adding an organic substance or an acid to an aqueous solution of an alkali salt of ruthenium acid prepared by dissolving or melting ruthenium metal in an alkali.
【０００３】[0003]
【発明が解決しようとする課題】しかし、上記方法で
は、湿式で微粒子の沈殿を形成し、しかもその後熱処理
をするため粒子同士の凝集が強く、ペースト中に均一に
分散させることが困難であるとともに、結果として厚膜
抵抗体の特性の向上には限界があるという問題点があ
る。本発明の目的は、凝集が弱く分散性に優れ、かつ厚
膜抵抗体用として優れた特性を持つ二酸化ルテニウム微
粉末の製造方法の提供にある。However, in the above method, since the fine particles are formed by a wet method and heat treatment is performed thereafter, the particles are strongly aggregated with each other, and it is difficult to uniformly disperse them in the paste. As a result, there is a limit in improving the characteristics of the thick film resistor. An object of the present invention is to provide a method for producing a ruthenium dioxide fine powder having weak aggregation, excellent dispersibility, and excellent properties for thick film resistors.
【０００４】[0004]
【課題を解決するための手段】本発明者は上記問題点を
解決するために種々の検討を行った結果、本発明に至っ
た。すなわち、上記課題を解決する本発明の方法は、９
５重量部以下のルテニウム酸鉛微粉末とＢ2 Ｏ3 換算で
５重量部以上の酸化硼素または硼酸とを混合し、該混合
物を７００℃以上の温度で溶融したのち、該溶融物を純
水または酸に溶解して得た沈殿を濾過、洗浄、乾燥する
ことを特徴とする二酸化ルテニウム微粉末の製造方法で
ある。The present inventor has accomplished the present invention as a result of various studies to solve the above problems. That is, the method of the present invention for solving the above problems is
5 parts by weight or less of lead ruthenate fine powder and 5 parts by weight or more of boron oxide or boric acid in terms of B 2 O 3 are mixed, and the mixture is melted at a temperature of 700 ° C. or more, and the melt is purified water. Alternatively, the method is a method for producing a ruthenium dioxide fine powder, which comprises filtering, washing and drying a precipitate obtained by dissolving in an acid.
【０００５】[0005]
【作用】本発明者は種々の検討を行った結果、ルテニウ
ム酸鉛を酸化硼素共存下で加熱すると、ルテニウム酸鉛
は二酸化ルテニウムと酸化鉛に分解し、硼酸鉛ガラス中
に二酸化ルテニウムが分散した状態となることを見出
し、本発明に至った。ルテニウム酸鉛と混合する酸化硼
素または硼酸の割合をＢ2 Ｏ3 換算で５重量部以上とし
たのは、５重量部未満ではルテニウム酸鉛の分解が不十
分であり、ルテニウム酸鉛が残存するので良くないから
である。また、溶融温度を７００℃以上としたのは、溶
融温度が７００℃未満では、ルテニウム酸鉛の分解が不
十分であり、ルテニウム酸鉛が残存するので良くないか
らである。該溶融物は硼酸鉛ガラス中に二酸化ルテニウ
ムが分散した状態となっているものであり、純水望まし
くは酢酸水溶液等の弱酸で硼酸鉛ガラスを溶解すれば濾
過等により容易に二酸化ルテニウムを回収することがで
きる。その後、純水で洗浄、乾燥することにより凝集の
弱い分散性に優れた二酸化ルテニウム微粉末が得られ
る。As a result of various investigations by the present inventor, when lead ruthenate was heated in the presence of boron oxide, the lead ruthenate was decomposed into ruthenium dioxide and lead oxide, and the ruthenium dioxide was dispersed in the lead borate glass. The present invention has been accomplished by discovering that a state is brought about. The ratio of boron oxide or boric acid mixed with lead ruthenate is 5 parts by weight or more in terms of B 2 O 3 because less than 5 parts by weight lead ruthenate is not sufficiently decomposed and lead ruthenate remains. Because it is not good. The reason why the melting temperature is 700 ° C. or higher is that if the melting temperature is lower than 700 ° C., the decomposition of lead ruthenate is insufficient and lead ruthenate remains, which is not preferable. The melt is a state in which ruthenium dioxide is dispersed in lead borate glass, and if ruthenium dioxide is dissolved in pure water, preferably a weak acid such as an acetic acid aqueous solution, ruthenium dioxide is easily recovered by filtration or the like. be able to. Then, by washing with pure water and drying, ruthenium dioxide fine powder with weak aggregation and excellent dispersibility can be obtained.
【０００６】[0006]
（実施例１）ルテニウム酸鉛粉末２７ｇと酸化硼素粉末
１０ｇとをめのう製のらいかい機で３０分間混合した
後、該混合物をアルミナるつぼに入れて８００℃の温度
で１時間溶融した。次に、該溶融物を取り出し、酢酸の
１０％水溶液５００ｃｃに溶解した後、濾過、洗浄し、
１１０℃で一晩乾燥して９．５ｇの二酸化ルテニウム微
粉末が得られた。この微粉末を透過型電子顕微鏡で観察
したところいずれも５００〜１０００Åの粒径であっ
た。この二酸化ルテニウム微粉末１５重量部とＰｂＯ−
ＳｉＯ2 −Ｂ2 Ｏ3 −Ａｌ2 Ｏ3 系ガラス５５重量部と
樹脂分エチルセルロースと溶剤ターピネオールよりなる
ビヒクル３０重量部とを混合してペーストを作成し、該
ペーストを印刷し、ピーク８５０℃×９分、トータル３
０分のベルト炉で焼成して作成した長さ１ｍｍ、幅１ｍ
ｍ、厚さ８μｍの厚膜抵抗体の電気的性能を測定した。
結果は、抵抗値が８９０ｋΩ／□、抵抗値の変動率が
３．７％、ノイズが−６ｄＢであった。(Example 1) 27 g of lead ruthenate powder and 10 g of boron oxide powder were mixed for 30 minutes by an agate-made raft machine, and then the mixture was put into an alumina crucible and melted at a temperature of 800 ° C. for 1 hour. Next, the melt was taken out, dissolved in 500 cc of a 10% aqueous solution of acetic acid, filtered, washed,
After drying at 110 ° C. overnight, 9.5 g of ruthenium dioxide fine powder was obtained. When the fine powder was observed with a transmission electron microscope, all had a particle size of 500 to 1000Å. 15 parts by weight of this ruthenium dioxide fine powder and PbO-
55 parts by weight of SiO 2 —B 2 O 3 —Al 2 O 3 based glass and 30 parts by weight of a vehicle composed of resin component ethyl cellulose and a solvent terpineol were mixed to form a paste, the paste was printed, and the peak was 850 ° C. × 9 minutes, total 3
1 mm long and 1 m wide created by firing in a belt furnace for 0 minutes
The electrical performance of a thick film resistor having a thickness of m and a thickness of 8 μm was measured.
As a result, the resistance value was 890 kΩ / □, the variation rate of the resistance value was 3.7%, and the noise was −6 dB.
【０００７】（実施例２）ルテニウム酸鉛と酸化硼素と
の混合割合および溶融条件を変えて実施例１と同様にし
て粉末を作成した。その結果を表１に示した。Example 2 A powder was prepared in the same manner as in Example 1, except that the mixing ratio of lead ruthenate and boron oxide and the melting conditions were changed. The results are shown in Table 1.
【０００８】（比較例）ルテニウム酸鉛と酸化硼素との
混合割合および溶融条件を変えて実施例１と同様にして
粉末を作成した。その結果を表１に合わせて示した。Comparative Example A powder was prepared in the same manner as in Example 1 except that the mixing ratio of lead ruthenate and boron oxide and the melting conditions were changed. The results are also shown in Table 1.
【０００９】[0009]
【表１】 [Table 1]
【００１０】[0010]
【発明の効果】本発明の方法によれば、厚膜抵抗ペース
トの材料として好ましい凝集の弱い分散性に優れた二酸
化ルテニウム微粉末を得ることができる。According to the method of the present invention, it is possible to obtain ruthenium dioxide fine powder having a weak aggregation and excellent dispersibility, which is preferable as a material for a thick film resistance paste.
Claims (1)
とＢ2 Ｏ3 換算で５重量部以上の酸化硼素または硼酸と
を混合し、該混合物を７００℃以上の温度で溶融したの
ち、該溶融物を純水または酸に溶解して得た沈殿を濾
過、洗浄、乾燥することを特徴とする二酸化ルテニウム
微粉末の製造方法。1. 95 parts by weight or less of lead ruthenate fine powder and 5 parts by weight or more of boron oxide or boric acid in terms of B 2 O 3 are mixed, and the mixture is melted at a temperature of 700 ° C. or more, A method for producing a ruthenium dioxide fine powder, which comprises filtering, washing and drying a precipitate obtained by dissolving a melt in pure water or an acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19187693A JPH0725620A (en) | 1993-07-07 | 1993-07-07 | Production of ruthenium dioxide fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19187693A JPH0725620A (en) | 1993-07-07 | 1993-07-07 | Production of ruthenium dioxide fine powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0725620A true JPH0725620A (en) | 1995-01-27 |
Family
ID=16281950
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19187693A Pending JPH0725620A (en) | 1993-07-07 | 1993-07-07 | Production of ruthenium dioxide fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0725620A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013053030A (en) * | 2011-09-02 | 2013-03-21 | Sumitomo Metal Mining Co Ltd | Plate-like ruthenium oxide powder, method for producing the same, and thick film resistor composition using the same |
| WO2013168339A1 (en) | 2012-05-10 | 2013-11-14 | 株式会社大真空 | Piezoelectric device |
-
1993
- 1993-07-07 JP JP19187693A patent/JPH0725620A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2013053030A (en) * | 2011-09-02 | 2013-03-21 | Sumitomo Metal Mining Co Ltd | Plate-like ruthenium oxide powder, method for producing the same, and thick film resistor composition using the same |
| WO2013168339A1 (en) | 2012-05-10 | 2013-11-14 | 株式会社大真空 | Piezoelectric device |
| US9893711B2 (en) | 2012-05-10 | 2018-02-13 | Daishinku Corporation | Piezoelectric device |
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