JPH01257136A - Lead ruthenate fine powder for electrically conductive material, thick film resister paste containing same and production of lead ruthenate fine powder - Google Patents
Lead ruthenate fine powder for electrically conductive material, thick film resister paste containing same and production of lead ruthenate fine powderInfo
- Publication number
- JPH01257136A JPH01257136A JP63085989A JP8598988A JPH01257136A JP H01257136 A JPH01257136 A JP H01257136A JP 63085989 A JP63085989 A JP 63085989A JP 8598988 A JP8598988 A JP 8598988A JP H01257136 A JPH01257136 A JP H01257136A
- Authority
- JP
- Japan
- Prior art keywords
- fine powder
- lead ruthenate
- lead
- thick film
- powder
- 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
- 239000000843 powder Substances 0.000 title claims abstract description 32
- 239000004020 conductor Substances 0.000 title claims abstract description 9
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 239000002245 particle Substances 0.000 claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 15
- 239000003513 alkali Substances 0.000 claims abstract description 8
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 8
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Substances [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 7
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims abstract description 7
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims abstract description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 239000011347 resin Substances 0.000 claims abstract description 5
- 229920005989 resin Polymers 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007787 solid Substances 0.000 claims abstract description 4
- 229910000027 potassium carbonate Inorganic materials 0.000 claims abstract description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 10
- 238000006386 neutralization reaction Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 229910002651 NO3 Inorganic materials 0.000 abstract 2
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 abstract 2
- 229910019891 RuCl3 Inorganic materials 0.000 abstract 2
- 229910020333 Pb2Ru2O6.5 Inorganic materials 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910021529 ammonia Inorganic materials 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 235000015320 potassium carbonate Nutrition 0.000 abstract 1
- 235000017550 sodium carbonate Nutrition 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 12
- 239000000047 product Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910052707 ruthenium Inorganic materials 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 239000001856 Ethyl cellulose Substances 0.000 description 1
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 1
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical group O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- FGEKTVAHFDQHBU-UHFFFAOYSA-N dioxoruthenium;hydrate Chemical compound O.O=[Ru]=O FGEKTVAHFDQHBU-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003304 ruthenium compounds Chemical class 0.000 description 1
- GTCKPGDAPXUISX-UHFFFAOYSA-N ruthenium(3+);trinitrate Chemical compound [Ru+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O GTCKPGDAPXUISX-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G55/00—Compounds of ruthenium, rhodium, palladium, osmium, iridium, or platinum
Abstract
Description
【発明の詳細な説明】
（産業上の利用分！）
本発明は厚膜抵抗体の導電材料として有用であるルテニ
ウム酸鉛微粉末及びこれを用いた厚膜抵抗体ペースト並
びに同微粉末の製造方法に関する。Detailed Description of the Invention (Industrial Applications!) The present invention relates to a lead ruthenate fine powder useful as a conductive material for thick film resistors, a thick film resistor paste using the same, and the production of the fine powder. Regarding the method.
（従来の技術）
従来、ルテニウム酸鉛微粉末の製造に際しては、例えば
、二酸化ルテニウム粉末と硝酸鉛粉末とを機械的に混合
し、これを熱処理した后に粉砕してルテニウム酸鉛の微
粉末を入手する乾式方法並びに酸素供給源の存在下にア
ルカリ性液体の媒体中でルテニウム化合物（硝酸ルテニ
ウム、ニトロシル等）と、鉛化合物とを反応させてルテ
ニウム酸鉛を得る湿式方法とに分けられている。(Prior art) Conventionally, when manufacturing lead ruthenate fine powder, for example, ruthenium dioxide powder and lead nitrate powder are mechanically mixed, and after heat treatment, the mixture is pulverized to produce fine lead ruthenate powder. It is divided into a dry method for obtaining lead ruthenate, and a wet method for obtaining lead ruthenate by reacting a ruthenium compound (ruthenium nitrate, nitrosyl, etc.) with a lead compound in an alkaline liquid medium in the presence of an oxygen source.
また、ルテニウム酸鉛を厚膜抵抗体に用いる場合にはそ
のペースト特性に及ぼすルテニウム酸鉛の製品粒度が極
めて大きな影響力を示すもので粒子径が５００Å以上、
１０００Å以下であって、粒度分布の狭い分散性の良好
な粉末が好ましいと云われてる。In addition, when lead ruthenate is used for thick film resistors, the particle size of the lead ruthenate product has a very large influence on the paste characteristics, and the particle size is 500 Å or more.
It is said that a powder with a particle diameter of 1000 Å or less, a narrow particle size distribution, and good dispersibility is preferable.
（発明が解決しようとする課題）
然し乍ら、前記の乾式法による場合には、粒径の小さな
製品が得られ難く、しかも未反応の酸化鉛及び二酸化ル
テニウムが残存してしまう確率が高くなり、一方前記湿
式法で得られるものは１００人程鹿の超微粒子である為
、触媒等には有効であるが、厚膜抵抗体に用いるペース
ト用にはそのま１の形状に於いて用いるには粒径が小さ
すぎて分散しにくいと云う解決すべき課題が夫々残され
ている。(Problems to be Solved by the Invention) However, when using the dry method described above, it is difficult to obtain a product with a small particle size, and there is a high probability that unreacted lead oxide and ruthenium dioxide will remain. The particles obtained by the wet method are ultrafine particles of about 100 particles, which are effective for catalysts, etc., but the particles are too small to be used in their original form for pastes used in thick film resistors. There remains a problem to be solved, namely that the diameter is too small and it is difficult to disperse.
（課題を解決するための手段）
本発明者は、上記した如き従来の技術による場合の課題
解決のため種々研究実験の結果下達する新しい湿式方法
によって５００〜１０００人の粒径範囲を持ちその微粉
末の殆どがＰｂ２Ｒｕ２Ｏ６゜で表わされるルテニウム
酸鉛よりなる導電材料用のルテニウム酸鉛微粉末をこ１
に提供するものであり、これと同時に同微粉末の高電気
抵抗、抵抗値のバラツキの低さ及び低ノイズを利用した
厚膜抵抗体ペースト並びに上記微粉末の製造方法をこ１
に併せて提供するものである。即ち本発明は；Ｐｂ、Ｒ
ｕ２Ｏ，、、で表わされその粒径範囲が５００〜１００
０人の微粉末を主体とした導電材料用のルテニウム酸鉛
微粉末及び上記のルテニウム酸鉛微粉末１５〜４５重量
％及びＰｂＯ−５ｉｎ２−Ａ１２０．系ガラス５５〜８
５重量％からなる固形分、溶剤及び樹脂分より構成され
た厚膜抵抗体ペースト並びに次の工程ａ、ｂよりなる導
電材料用のルテニウム酸鉛微粉末の製造方法を夫々提供
するものである。(Means for Solving the Problems) In order to solve the problems with the conventional techniques as described above, the present inventor has developed a new method using a new wet method, which was developed as a result of various research experiments, to obtain particles in the particle size range of 500 to 1,000. This is a fine lead ruthenate powder for conductive materials, most of which is made of lead ruthenate expressed as Pb2Ru2O6°.
At the same time, the present invention provides a thick film resistor paste that takes advantage of the fine powder's high electrical resistance, low variation in resistance value, and low noise, as well as a method for producing the fine powder.
It will be provided in conjunction with. That is, the present invention; Pb, R
It is expressed as u2O,, and its particle size range is 500 to 100.
Lead ruthenate fine powder for conductive materials mainly composed of 0 people's fine powder and 15 to 45% by weight of the above lead ruthenate fine powder and PbO-5in2-A120. Series glass 55-8
The present invention provides a thick film resistor paste composed of a solid content of 5% by weight, a solvent and a resin content, and a method for producing fine lead ruthenate powder for conductive materials, which consists of the following steps a and b.
ａ、塩化ルテニウム及び硝酸鉛よりなる混合液と、アル
カリとを２５℃以上、１００℃以下の温度範囲で反応さ
せて中和共沈させる中和工程、及び
ｂ．上記中和工程に於て沈澱生成した沈澱物を洗浄、濾
過及び乾燥の后７００℃以上、８００℃以下にて加熱焼
成する熱処理工程。a. A neutralization step of reacting a mixed solution of ruthenium chloride and lead nitrate with an alkali at a temperature range of 25° C. or higher and 100° C. or lower to neutralize and coprecipitate; and b. A heat treatment step in which the precipitate formed in the neutralization step is washed, filtered, and dried, and then heated and calcined at a temperature of 700° C. or more and 800° C. or less.
前記ルテニウム酸鉛微粉末の特長ある性状、物性に関し
ては上記の製造方法の説明より明らかになると思うの製
造方法を先立って説明するものである。The manufacturing method will be explained first, since the characteristic properties and physical properties of the fine lead ruthenate powder will become clear from the above description of the manufacturing method.
上記の製造方法に用いられるアルカリは、水酸化ナトリ
ウム、水酸化カリウム、アンモニア水、炭酸ソーダ及び
炭酸カリウム等である。The alkali used in the above production method includes sodium hydroxide, potassium hydroxide, aqueous ammonia, soda carbonate, potassium carbonate, and the like.
また、中和反応は２５℃以上１００℃以下の温度範囲で
行なうが、より好ましくは４０℃以上８０℃以下の温度
範囲である。Further, the neutralization reaction is carried out at a temperature range of 25°C or higher and 100°C or lower, more preferably a temperature range of 40°C or higher and 80°C or lower.
（作用）
本発明では塩化ルテニウム及び硝酸鉛からなる混合液と
、アルカリとを２５〜１００℃の温度範囲で中和させて
中和共沈させて、この中和工程で沈澱生成した沈澱物を
洗浄、濾過及び乾燥の后７００℃〜８００℃で加熱焙焼
することによりｐｂ、Ｒｕ、Ｏ，、で表わされるルテニ
ウム酸鉛の単相よりなる微粉末を高収率（９８，５％）
をもって得ることが出来るのである。(Function) In the present invention, a mixed solution consisting of ruthenium chloride and lead nitrate and an alkali are neutralized at a temperature range of 25 to 100°C to cause neutralization coprecipitation, and the precipitate formed in this neutralization step is removed. After washing, filtration and drying, the fine powder consisting of a single phase of lead ruthenate represented by pb, Ru, O, etc. is produced in high yield (98.5%) by heating and roasting at 700°C to 800°C.
It can be obtained with.
上記中和反応に於ける詳細な反応式について発明者は充
分な反応式を解明することは出来ないが、上述の温度範
囲の限定理由については反応の実際より以下に説明する
ことが出来る。Although the inventors are unable to fully elucidate the detailed reaction formula for the above neutralization reaction, the reason for limiting the above-mentioned temperature range can be explained below from the actual reaction.
上記に於て、塩化ルテニウム及び硝酸鉛からなる混合液
と、アルカリとを２５℃以上１００°Ｃ以下の温度範囲
にて反応させるのは、２５℃未満では生成する粒子が大
きく凝集してしまい、１００℃を超える場合には特に顕
著な効果が見られぬばかりか、加熱に費される熱エネル
ギーの損失が高くなる為である。In the above, the reason why the mixed solution consisting of ruthenium chloride and lead nitrate is reacted with an alkali at a temperature range of 25°C or higher and 100°C or lower is that if the temperature is lower than 25°C, the particles produced will greatly aggregate. This is because when the temperature exceeds 100° C., not only no remarkable effect is observed, but also the loss of thermal energy used for heating increases.
又、中和工程で生成した沈澱物を７００℃以上、８００
℃以下にて粉末の焙焼を目的として加熱するのは、７０
０℃未満では二酸化ルテニウム（ＲｕＯ２）の割合が多
くなると共に一般式Ｐｂ２（ＲＬ１２−５ Ｐｂａ ）
０７−Ｘで表わされるルテニウム酸鉛も存在して製品の
純度を落してしまう為であり、８００℃を超えると粒子
の成長が激しく、微細な粒子が得難くなる為である。In addition, the precipitate generated in the neutralization process was heated to 700°C or higher and 800°C.
Heating for the purpose of roasting powder at temperatures below 70℃
Below 0°C, the proportion of ruthenium dioxide (RuO2) increases and the general formula Pb2 (RL12-5 Pba)
This is because the presence of lead ruthenate represented by 07-X reduces the purity of the product, and when the temperature exceeds 800°C, particle growth is rapid and it becomes difficult to obtain fine particles.
熱処理に於ける通常の概念として、その効果は物体に加
えられる熱量の合計で判断されるものではあるが、本発
明の場合粉末焙焼作業が請求項３に規定した温度に対し
て低温度長時間でも、高温度長時間でも好ましい結果は
みられず何れも二酸化ルテニウムの割合が高くなると共
にＰｂ、（ＲＵっＰｂ１）Ｏ□−叉が残存して、製品の
純度を下げる結果を示す。As a general concept in heat treatment, the effect is judged by the total amount of heat added to the object, but in the case of the present invention, the powder roasting operation is carried out at a low temperature for a long time compared to the temperature specified in claim 3. No favorable results were observed either in terms of time or high temperature for a long period of time; in both cases, the proportion of ruthenium dioxide increased and Pb, (RU-Pb1)O□- remained, reducing the purity of the product.
例えば９００℃で２０分を越えた焙焼処理を行なうと急
激な粒成長を生じて目的をはたす事が出来なくなる。一
方、６００℃近傍にて焙焼処理された製品はＸ線回折に
よる観察によるとＰ ｂ２Ｒｕ ２０６．、と、Ｒｕｂ
、と、Ｐ ｂ、 （Ｒｕ、−Ｉ Ｐｂ３− ）０６、シ
との混合物と認められるに対し、本発明の７００℃以上
、８００℃以下に焙焼処理された粉末はＰｂ、Ｒｕ、○
５．．のみしか生成しない。For example, if the roasting treatment is carried out at 900° C. for more than 20 minutes, rapid grain growth will occur and the purpose will not be achieved. On the other hand, the product roasted at around 600°C has P b2Ru 206% as observed by X-ray diffraction. , and Rub
, Pb, (Ru, -I Pb3-)06, and Pb, (Ru, -IPb3-)06, and Pb, (Ru, -IPb3-)06, and Pb, (Ru, -I Pb3-)06, and Pb, (Ru, -I Pb3-), whereas the powder roasted at 700°C or higher and 800°C or lower according to the present invention contains Pb, Ru,
5. ．． It only generates
（実施例）
塩化ルテニウム０．２ｍｏ１．硝酸鉛Ｑ、２ｍｏｌに純
水を加えて１２００ｍ１とし、６５℃にて加熱攪拌しつ
つこの溶液に６５℃にて加熱した１、４ｍ。(Example) Ruthenium chloride 0.2mol. Pure water was added to 2 mol of lead nitrate Q to make 1200 ml, and 1.4 ml of this solution was heated at 65° C. while stirring.
１／ＩＩＩの水酸化ナトリウム溶液８００ｍ１を添加し
て黒色沈澱物を生成せしめ、この黒色沈澱物を温水で洗
浄濾過したのち１００℃にて乾燥した。800 ml of 1/III sodium hydroxide solution was added to form a black precipitate, which was washed and filtered with warm water and then dried at 100°C.
次いで、７５０℃にて２時間の熱処理を加えた場合、生
成した粉末をＸ線回折法により調査した結果、Ｐ ｂ
２ Ｒｕ ｚ Ｏｓ、ｓの単相である事が判明した。Next, when heat treatment was applied at 750°C for 2 hours, the resulting powder was examined by X-ray diffraction, and as a result, P b
It turned out to be a single phase of 2 Ru z Os,s.
又、この粉末を透過電子顕微鏡で１０万倍に拡大して観
察した結果、その平均粒径は５００〜１０００人と比較
的揃った粒径の製品であり、収率は９８．５％に及んだ
。又、用いるＮａＯＨより移行するＮａの含有量は０．
０１重量％以下と極めて低い値を示したにすぎなかった
。これは従来法としての湿式法による場合の粒径１００
人未満と比較してはるかに大きく厚膜抵抗体の導電材料
として最も好ましい粒度分布になっていた。Furthermore, when this powder was observed under a transmission electron microscope at a magnification of 100,000 times, it was found that the product had a relatively uniform average particle size of 500 to 1000 people, and the yield was 98.5%. I did. Moreover, the content of Na transferred from the NaOH used is 0.
It showed an extremely low value of 0.01% by weight or less. This is the particle size of 100 when using the conventional wet method.
The particle size distribution was much larger than that of a human particle, making it the most preferable particle size distribution for a conductive material for thick film resistors.
又、この粉末を用いてＰｂ、Ｒｕ、０６．、を２０重量
％、Ｐ ｂ Ｏ−Ｓ ｉ ０２−Ａ １．０３系ガラス
を５０重量％、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イクルを３０重量％の割合で製造し
たペーストを用いてピークで８５０℃×９分、合計５０
分の加熱焙焼をした場合の１０μｎａＸ１ｍｍＸ１ｍｍ
の厚膜抵抗体について電気抵抗を測定した結果は抵抗値
が４．３にΩ、抵抗値のバラツキ２．７％、 ノイズ−
１１ドルビーであった。Also, using this powder, Pb, Ru, 06. , 20% by weight of P b O-S i 02-A 1.03 glass, 30% by weight of a vehicle consisting of ethyl cellulose as a resin and terpineol as a solvent. 850℃ x 9 minutes, total 50
10μnaX1mmX1mm when heated and roasted for minutes
As a result of measuring the electrical resistance of the thick film resistor, the resistance value was 4.3 Ω, the variation in resistance value was 2.7%, and the noise was -
It was 11 dolbys.
（比較例）
本発明と比較の為に用意した二酸化ルテニウム水和物と
ｐｂ （Ｎｏｉ）ｚ とをライカイ機で３０分間混合し
て６００℃で２時間の焙焼処理をした粉末を用いて他は
実施例と同様な方法で作成したペーストについての試験
を行ない１０μ＠ＸＸｌｍｍＸ１ａの厚膜抵抗体につい
て電気抵抗を測定した結果は抵抗値が２．８にΩ、抵抗
値のバラツキ８．５％、ノイズ＋１３ドルビーであった
。(Comparative Example) A powder obtained by mixing ruthenium dioxide hydrate and pb (Noi)z prepared for the purpose of comparison with the present invention for 30 minutes in a Raikai machine and roasting the mixture at 600°C for 2 hours was used. conducted a test on a paste prepared in the same manner as in the example, and measured the electrical resistance of a thick film resistor of 10μ@XXlmmX1a.The results showed that the resistance value was 2.8Ω, and the variation in resistance was 8.5%. It was noise + 13 Dolby.
以上から明らかな如く、本発明によるルテニウム酸鉛を
用いる時は、厚膜抵抗体作成用のペーストの特性も大幅
に向上する事が可能となった。As is clear from the above, when the lead ruthenate according to the present invention is used, the characteristics of the paste for producing a thick film resistor can be significantly improved.
なお、厚膜抵抗体ペーストを得るについて前記実施例の
他にルテニウム酸鉛微粉末１５〜４５重量％及びｐ ｂ
Ｏ−８ｉ Ｏ，−Ａ ｌ、ｏ３系ガラス５５〜８５重
量％からなる固形分、溶剤及び樹脂分から構成すること
が８来る。In order to obtain the thick film resistor paste, in addition to the above examples, 15 to 45% by weight of lead ruthenate fine powder and pb
O-8i O, -Al, solid content consisting of 55 to 85% by weight of O3 glass, solvent and resin.
（発明の効果）
本発明による時は、電子機器業界に於いて広く用いられ
ている厚膜抵抗体に用いるペースト材料としてのルテニ
ウム酸鉛として最も好ましい粉子粒径の５００〜１００
０人が収率高く得られ、更に二酸化ルテニウム等の不純
物の存在が極めて低い製品を入手する事が可能になり業
界に寄与するところ極めて大なるものがある。(Effects of the Invention) According to the present invention, the powder particle size is 500 to 100, which is the most preferable lead ruthenate as a paste material used in thick film resistors widely used in the electronic equipment industry.
This makes it possible to obtain a product with a high yield and an extremely low presence of impurities such as ruthenium dioxide, which will greatly contribute to the industry.
Claims (4)
径範囲が５００〜１０００Åの微粉末を主体とした導電
材料用のルテニウム酸鉛微粉末。1. Pb_2Ru_2O_6_. Lead ruthenate fine powder for conductive materials, which is represented by _5 and whose particle size range is 500 to 1000 Å.
及びＰｂＯ−ＳｉＯ＿２−Ａｌ＿２Ｏ＿３系ガラス５５
〜８５重量％からなる固形分、溶剤及び樹脂分より構成
された厚膜抵抗体ペースト。2. 15 to 45% by weight of lead ruthenate fine powder according to claim 1
and PbO-SiO_2-Al_2O_3 glass 55
A thick film resistor paste composed of a solid content of ~85% by weight, a solvent, and a resin content.
鉛微粉末の製造方法。 ａ．塩化ルテニウム及び硝酸鉛よりなる混合液と、アル
カリとを２５℃以上、１００℃以下の温度範囲で反応さ
せて中和共沈させる中和工程、及び ｂ．上記中和工程に於て沈澱生成した沈澱物を洗浄、濾
過及び乾燥の后７００℃以上、８００℃以下にて加熱焙
焼する熱処理工程。3. A method for producing fine lead ruthenate powder for conductive materials, comprising the following steps a and b. a. a neutralization step of reacting a mixed solution of ruthenium chloride and lead nitrate with an alkali at a temperature range of 25° C. or higher and 100° C. or lower to neutralize and coprecipitate; and b. A heat treatment step in which the precipitate formed in the neutralization step is washed, filtered, and dried, and then heated and roasted at a temperature of 700° C. or more and 800° C. or less.
ンモニア水、炭酸ソーダ及び炭酸カリウムのいづれかよ
り選ばれたものである請求項３記載の製造方法。4. 4. The method according to claim 3, wherein the alkali is selected from sodium hydroxide, potassium hydroxide, aqueous ammonia, sodium carbonate, and potassium carbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63085989A JPH01257136A (en) | 1988-04-07 | 1988-04-07 | Lead ruthenate fine powder for electrically conductive material, thick film resister paste containing same and production of lead ruthenate fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63085989A JPH01257136A (en) | 1988-04-07 | 1988-04-07 | Lead ruthenate fine powder for electrically conductive material, thick film resister paste containing same and production of lead ruthenate fine powder |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01257136A true JPH01257136A (en) | 1989-10-13 |
Family
ID=13874086
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63085989A Pending JPH01257136A (en) | 1988-04-07 | 1988-04-07 | Lead ruthenate fine powder for electrically conductive material, thick film resister paste containing same and production of lead ruthenate fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01257136A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010092971A1 (en) * | 2009-02-10 | 2010-08-19 | 新日本石油株式会社 | Process for preparing pyrochlore oxide, and polymer electrolyte membrane fuel cell, fuel cell system, and process for producing electrode catalyst for fuel cell |
| JP2020193138A (en) * | 2019-05-30 | 2020-12-03 | 住友金属鉱山株式会社 | Method for producing lead ruthenate powder, lead ruthenate powder, and thick film resistor paste containing lead ruthenate powder |
-
1988
- 1988-04-07 JP JP63085989A patent/JPH01257136A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010092971A1 (en) * | 2009-02-10 | 2010-08-19 | 新日本石油株式会社 | Process for preparing pyrochlore oxide, and polymer electrolyte membrane fuel cell, fuel cell system, and process for producing electrode catalyst for fuel cell |
| JP2010184824A (en) * | 2009-02-10 | 2010-08-26 | Nippon Oil Corp | Method for preparing pyrochlore type oxide, polymer electrolyte fuel cell, fuel cell system and method for producing electrode catalyst for fuel cell |
| US8329129B2 (en) | 2009-02-10 | 2012-12-11 | Jx Nippon Oil & Energy Corporation | Method for preparing pyrochlore oxide, polymer electrolyte fuel cell, fuel cell system, and method for producing electro catalyst for fuel cell |
| JP2020193138A (en) * | 2019-05-30 | 2020-12-03 | 住友金属鉱山株式会社 | Method for producing lead ruthenate powder, lead ruthenate powder, and thick film resistor paste containing lead ruthenate powder |
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