JPH02302327A - Production of lead ruthenate fine powder - Google Patents
Production of lead ruthenate fine powderInfo
- Publication number
- JPH02302327A JPH02302327A JP12045289A JP12045289A JPH02302327A JP H02302327 A JPH02302327 A JP H02302327A JP 12045289 A JP12045289 A JP 12045289A JP 12045289 A JP12045289 A JP 12045289A JP H02302327 A JPH02302327 A JP H02302327A
- Authority
- JP
- Japan
- Prior art keywords
- solution
- lead
- fine powder
- precipitates
- ruthenium
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000002244 precipitate Substances 0.000 claims abstract description 18
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 11
- 150000002500 ions Chemical class 0.000 claims abstract description 9
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 10
- 229910052707 ruthenium Inorganic materials 0.000 claims description 10
- 239000003513 alkali Substances 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 239000007800 oxidant agent Substances 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims 1
- 239000000243 solution Substances 0.000 abstract description 27
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 10
- 239000012670 alkaline solution Substances 0.000 abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 229910017604 nitric acid Inorganic materials 0.000 abstract description 4
- 239000007788 liquid Substances 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract description 3
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 229910020333 Pb2Ru2O6.5 Inorganic materials 0.000 abstract 1
- 238000001354 calcination Methods 0.000 abstract 1
- 239000007787 solid Substances 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 9
- 239000004020 conductor Substances 0.000 description 5
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 3
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 description 3
- 239000005708 Sodium hypochlorite Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000002611 lead compounds Chemical class 0.000 description 2
- 229910000464 lead oxide Inorganic materials 0.000 description 2
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 150000003304 ruthenium compounds Chemical class 0.000 description 2
- 239000011163 secondary particle Substances 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 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
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 230000003113 alkalizing effect Effects 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
- 150000001450 anions Chemical class 0.000 description 1
- 239000007864 aqueous solution Substances 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
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920001249 ethyl cellulose Polymers 0.000 description 1
- 235000019325 ethyl cellulose Nutrition 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 description 1
- VNZYIVBHUDKWEO-UHFFFAOYSA-L lead(ii) hydroxide Chemical compound [OH-].[OH-].[Pb+2] VNZYIVBHUDKWEO-UHFFFAOYSA-L 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 229940116411 terpineol Drugs 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】
［産業上の利用分野］
本発明は、厚膜抵抗体の導電物として有用であるルテニ
ウム酸鉛微粉末の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing fine lead ruthenate powder useful as a conductor for thick film resistors.
［従来の技術］
空気中等酸化雰囲気で焼成される抵抗体厚膜用の抵抗ペ
ーストには、導電物として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。[Prior Art] Ruthenium oxide fine powder or lead ruthenate fine powder is used as a conductive material in a resistance paste for a thick film of a resistor which is fired in an oxidizing atmosphere such as air.
一般に酸化ルテニウムは、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。Generally, ruthenium oxide is used as a conductive material with a wide range of resistance values, from low resistance values to high resistance values, and lead ruthenate is used as a conductive material with a high resistance value.
また、ルテニウム酸鉛は高抵抗領域において、導電物濃
度に対する抵抗値の変動率が酸化ルテニウムより小さく
、抵抗値の変動率の少ない抵抗体厚膜を製造することが
できる。更に、短時間過負荷（Ｓｈｏｒｔ Ｔｉｍｅ
０ｖｅｒ Ｌｏｒａｄ、略称５ＴＯＬ） や静電気破
壊（Ｅｌｅｃｔｒｏ ５ｔａｔｉｃ Ｄｉｓｃｈａｒｇ
ｅ、略称ＥＳＤ）による厚膜の永久抵抗値変化率が酸化
ルテニウムより小さく耐電圧性が優れている。このため
、抵抗ネットワーク用、チップ抵抗器用及びハイブリッ
ドＩＣの抵抗体厚膜用など電気回路の部品を形成する抵
抗ペーストの導電物粉末原料として広く利用されている
。これらのルテニウム酸鉛粉末は、粒子径や粒径分布の
小さな微粉末が用いられている。In addition, lead ruthenate has a smaller rate of variation in resistance value with respect to conductive material concentration than ruthenium oxide in a high resistance region, making it possible to produce a thick resistor film with a smaller rate of variation in resistance value. Furthermore, short time overload (Short Time
0ver Lorad, abbreviated as 5TOL) and electrostatic breakdown (Electro 5tatic Discharg).
The rate of change in the permanent resistance value of thick films due to ruthenium oxide (ESD) is smaller than that of ruthenium oxide, and it has excellent voltage resistance. For this reason, it is widely used as a conductive powder raw material for resistance pastes that form parts of electrical circuits, such as resistor networks, chip resistors, and thick film resistors of hybrid ICs. These lead ruthenate powders are fine powders with a small particle size and particle size distribution.
ところで、ルテニウム酸鉛を得る従来方法としては、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、
これを熱処理した後に粉砕してルテニウム酸鉛の微粉末
を得る乾式方法や、塩化ルテニウムとアルカリを混合し
、硝酸鉛をこれに添加し、次いで硝酸等を加えて加水分
解させるといった方法や、酸素供給源の存在下にアルカ
リ性溶液中でルテニウム化合物と鉛化合物とを反応させ
てルテニウム酸鉛を得るといった湿式方法がある。By the way, the conventional method for obtaining lead ruthenate is to mechanically mix ruthenium dioxide powder and lead nitrate powder,
There is a dry method in which ruthenium chloride is mixed with an alkali, lead nitrate is added thereto, and then nitric acid is added to hydrolyze it. There is a wet method in which lead ruthenate is obtained by reacting a ruthenium compound with a lead compound in an alkaline solution in the presence of a source.
Ｃ発明が解決しようとする課題］
しかし、上記乾式方法では粒径の小さなものが得られに
くく、しかも未反応の酸化鉛や二酸化ルテニウムが残存
してしまい。また湿式法では、例えば、塩化ルテニウム
とアルカリを混合し、この溶液に硝酸鉛を添加し、次い
で硝酸等を加えて鉛を加水分解するといった方法では、
塩化ルテニウムとアルカリとにより生じた含水酸化ルテ
ニウムスラリーに硝酸鉛を添加すると一時的に塩化鉛の
沈殿が生じ、この塩化鉛の一部が含水酸化ルテニウムの
沈殿に吸着等により取込まれ、得られる最終製品の性能
が低下するという問題点がある。Problems to be Solved by Invention C] However, in the dry method described above, it is difficult to obtain particles with a small particle size, and unreacted lead oxide and ruthenium dioxide remain. In the wet method, for example, ruthenium chloride and an alkali are mixed, lead nitrate is added to this solution, and then nitric acid is added to hydrolyze the lead.
When lead nitrate is added to the hydrous ruthenium oxide slurry produced from ruthenium chloride and an alkali, lead chloride precipitates temporarily, and a portion of this lead chloride is absorbed into the hydrous ruthenium oxide precipitate by adsorption, etc. There is a problem that the performance of the final product deteriorates.
また、例えば、酸素供給源の存在下にアルカリ性溶液中
でルテニウム化合物と鉛化合物とを反応させてルテニウ
ム酸鉛を得る方法では、得られる粉末が１００八程度の
超微粒子であるため、触媒等には有用であるが、厚膜抵
抗体に用いるペースト用としては凝集して大きさの異な
る二次粒子を形成し、かつ、ペースト中で均一に分散せ
ず、厚膜として焼成した場合に二次粒子が大きな結晶に
成長するという現象が見られるという問題点がある。In addition, for example, in the method of obtaining lead ruthenate by reacting a ruthenium compound and a lead compound in an alkaline solution in the presence of an oxygen supply source, the obtained powder is ultrafine particles of about 1008, so it is difficult to use as a catalyst. is useful for pastes used in thick film resistors, but it tends to aggregate to form secondary particles of different sizes, and is not uniformly dispersed in the paste, resulting in secondary particles forming when fired as a thick film. The problem is that particles tend to grow into large crystals.
本発明の目的は、５００〜ｔｏｏｏ Ａの粒径を持ち、
分散性がよく、かつ厚膜抵抗体として十分な特性を持つ
ルテニウム酸鉛微粉末の製造方法の提供にある。The object of the present invention is to have a particle size of 500 to too A,
An object of the present invention is to provide a method for producing fine lead ruthenate powder that has good dispersibility and sufficient characteristics as a thick film resistor.
［課題を解決するための手段］
本発明者らは上記問題点を解決するために種々の検討を
行なった結果、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金属ルテニウムを酸化剤共存下
でアルカリ溶解し、得タルテニウム酸溶液に、該溶液中
のルテニウムと当量の鉛イオンを含む溶液を添加して沈
殿を発生させ、得た沈殿を洗浄し、乾燥した後、６００
〜９００℃でばい焼することを特徴とするルテニウム酸
鉛微粉末の製造方法であり、好ましくは鉛イオンを含む
溶液として硝酸鉛溶液を用いるものであり、さらに好ま
しくは鉛イオンを含む溶液を添加した後、溶液のｐＨを
７〜９として沈殿を発生させるものである。[Means for Solving the Problems] The present inventors conducted various studies to solve the above problems, and as a result, they arrived at the present invention. That is, the method of the present invention for solving the above problems involves dissolving metal ruthenium in an alkali in the presence of an oxidizing agent, and adding a solution containing lead ions equivalent to the amount of ruthenium in the solution to the resulting tarthenic acid solution to cause precipitation. After generating, washing and drying the obtained precipitate, 600
A method for producing fine lead ruthenate powder characterized by baking at ~900°C, preferably using a lead nitrate solution as the solution containing lead ions, and more preferably adding a solution containing lead ions. After that, the pH of the solution is adjusted to 7 to 9 to generate a precipitate.
［作用］
本発明では金属ルテニウムを酸化剤共存下でアルカリ溶
解してルテニウム酸溶液を得るが、これは市販のルテニ
ウム酸塩は高襦で′あるばかりか、十分な純度のものが
ないためであり、さらに、反応を液・酸反応とすること
により生成する水酸化鉛あるいは酸化鉛と含水酸化ルテ
ニウムとが均一に混合した状態で共沈させるためである
。ルテニウム酸溶液を得る具体的な方法は、例えば金属
ルテニウムを水酸化ナトリウムと硝酸ナトリウムと混合
して溶融するものや、例えば水酸化ナトリウムと次亜塩
素酸ナトリウムの水溶液で溶解するものである。本発明
の方法において、使用するアルカリや酸化剤の量は金属
ルテニウムを完全に溶解できる量以上であればよい。[Function] In the present invention, a ruthenic acid solution is obtained by dissolving metallic ruthenium in an alkali in the presence of an oxidizing agent, but this is because commercially available ruthenic acid salts are not only high in purity, but also do not have sufficient purity. Furthermore, this is because lead hydroxide or lead oxide produced by conducting the reaction as a liquid/acid reaction and hydrated ruthenium oxide are co-precipitated in a uniformly mixed state. A specific method for obtaining a ruthenic acid solution is, for example, mixing metal ruthenium with sodium hydroxide and sodium nitrate and melting it, or dissolving it in an aqueous solution of sodium hydroxide and sodium hypochlorite, for example. In the method of the present invention, the amount of alkali or oxidizing agent used may be at least an amount that can completely dissolve metal ruthenium.
ルテニウム酸溶液に鉛イオンを含む溶液を加えたとき、
あまり ｐＨが高いとルテニウムや鉛が完全に沈殿せず
、収率を悪化させるため、要すれば溶液のｐＨを７〜９
に調節してルテニウム酸鉛を完全に沈殿させることが望
ましい。しかし、鉛イオンを含む溶液として硝酸鉛溶液
を用いれば、金属ルテニウムを溶解するのに大過剰のア
ルカリを用いていない限り、硝酸鉛溶液の添加後のｐＨ
は７〜９の範囲内になるので、特に［）Ｈの調整は要し
ない。When a solution containing lead ions is added to the ruthenic acid solution,
If the pH is too high, ruthenium and lead will not precipitate completely and the yield will deteriorate, so if necessary, lower the pH of the solution to 7 to 9.
It is desirable to completely precipitate lead ruthenate. However, if a lead nitrate solution is used as the solution containing lead ions, unless a large excess of alkali is used to dissolve the metal ruthenium, the pH after the addition of the lead nitrate solution will be
is within the range of 7 to 9, so no particular adjustment of [)H is required.
このようにして得られた沈殿は５００〜１０００Ａの微
粉末である。この沈殿中のアルカリ金属イオンや陰イオ
ンを除去するために洗浄し、次いでばい焼時の突沸現象
の発生を防止するために乾燥するが、この乾燥方法につ
いては特に限定されない。乾燥して得た沈殿よりルテニ
ウム酸鉛パイロクロア微粉末を製造するためには６００
〜９００゜Ｃの温度でばい焼することが必要である。The precipitate thus obtained is a fine powder of 500-1000A. The precipitate is washed to remove alkali metal ions and anions, and then dried to prevent the occurrence of bumping during roasting, but the drying method is not particularly limited. 600 to produce lead ruthenate pyrochlore fine powder from the precipitate obtained by drying.
It is necessary to bake at a temperature of ~900°C.
［実施例］
金属ルテニウム０．２ｍｏｌを次亜塩素酸ナトリウム（
有効塩素量１２％） ５００ ｍｌ水酸化ナトリウム５
０ｇ”を純水１０００ ｍｌに溶解して作成したアルカ
リ溶液に加え溶解しルテニウム酸溶液１５００ ＋ａｌ
を得た。一方、０．２ｍｏｌの硝酸鉛を１５％硝酸溶液
３００ ｍｌに溶解して硝酸鉛溶液３００ ｍｌを得た
。次いで、ルテニウム酸溶液１５００ ｍｌを６５℃に
維持し、攪はんしつつ、硝酸鉛溶液３００ｍ１を添加し
て黒色沈殿物を得た。この沈殿物を固液分離した後、温
水で洗浄し１１０℃で一晩乾燥した。[Example] 0.2 mol of metal ruthenium was added to sodium hypochlorite (
Available chlorine amount 12%) 500 ml Sodium hydroxide 5
0g" in 1000 ml of pure water to create an alkaline solution.
I got it. On the other hand, 0.2 mol of lead nitrate was dissolved in 300 ml of 15% nitric acid solution to obtain 300 ml of lead nitrate solution. Next, while maintaining 1500 ml of the ruthenic acid solution at 65° C. and stirring, 300 ml of lead nitrate solution was added to obtain a black precipitate. After solid-liquid separation of this precipitate, it was washed with warm water and dried at 110°C overnight.
このようにして得た黒色沈殿を８ｏｏ″Ｃで２時間ぽい
焼し酸化ルテニウムを含まないＰｂＪＬＩｉＯｓ、 ｓ
の組成式で表されるルテニウム酸鉛パイロクロア微粉末
が得られた。この微粉末を透過型電子顕微鏡で観察した
ところ何れも５００〜１０００ 、；の粒径であった。The black precipitate thus obtained was roasted at 80°C for 2 hours to give PbJLIiOs, which does not contain ruthenium oxide.
A fine powder of lead ruthenate pyrochlore represented by the composition formula was obtained. When this fine powder was observed with a transmission electron microscope, it was found that the particle size of each powder was 500 to 1,000.
なお、収率は９５．４％であり、ルテニウム酸鉛パイロ
クロア微粉末のナトリウム品位は０．０１重量％未満で
あった。The yield was 95.4%, and the sodium content of the lead ruthenate pyrochlore fine powder was less than 0.01% by weight.
このルテニウム酸鉛パイロクロア微粉末２６部とＰｂＯ
−５ｌｏｔ−ＡＩＪｓ系ガラス４４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部
とを混合してペーストを作成し、該ペーストを用いて作
成した長さ １ ｍｍ、幅１ ｍｍ’ｂ厚さ１２μｍの
厚膜抵抗体の電気的性能を測定した結果は抵抗値が８３
０Ω／口、抵抗値の変動率が２．３％、ノイズ−１５，
９ドルビーであった。26 parts of this lead ruthenate pyrochlore fine powder and PbO
A paste was prepared by mixing 44 parts of -5lot-AIJs glass and 30 parts of a vehicle consisting of ethyl cellulose as a resin and terpineol as a solvent, and a paste was prepared using the paste.Length: 1 mm, width: 1 mm'b, thickness: 12 μm As a result of measuring the electrical performance of the thick film resistor, the resistance value was 83.
0Ω/mouth, resistance fluctuation rate 2.3%, noise -15,
It was 9 Dolby.
［発明の効果］
本発明の方法によればペースト材料として好ましい粒径
５００〜１０００２の微細で均一なルテニウム酸鉛パイ
ロクロア微粉末を得ることができる。[Effects of the Invention] According to the method of the present invention, it is possible to obtain fine and uniform lead ruthenate pyrochlore fine powder with a particle size of 500 to 10,002, which is preferable as a paste material.
Claims (1)
得たルテニウム酸溶液に、該溶液中のルテニウムと当量
の鉛イオンを含む溶液を添加して沈殿を発生させ、得た
沈殿を洗浄し、乾燥した後、６００〜９００℃でばい焼
することを特徴とするルテニウム酸鉛微粉末の製造方法
。 ２、特許請求の範囲第１項記載のルテニウム酸鉛微粉末
の製造方法において、鉛イオンを含む溶液を添加した後
、溶液のｐＨを７〜９として沈殿を発生させることを特
徴とするルテニウム酸鉛微粉末の製造方法。 ３、鉛イオンを含む溶液として硝酸鉛溶液を用いること
を特徴とする特許請求の範囲第１〜２項記載のルテニウ
ム酸鉛微粉末の製造方法。[Claims] 1. Metal ruthenium is dissolved in an alkali in the presence of an oxidizing agent,
To the obtained ruthenic acid solution, a solution containing lead ions equivalent to the ruthenium in the solution is added to generate a precipitate, and the obtained precipitate is washed, dried, and then roasted at 600 to 900 ° C. Characteristic method for producing lead ruthenate fine powder. 2. The method for producing fine powder of lead ruthenate according to claim 1, characterized in that after adding a solution containing lead ions, the pH of the solution is adjusted to 7 to 9 to cause precipitation. A method for producing fine lead powder. 3. A method for producing fine lead ruthenate powder according to claims 1 to 2, characterized in that a lead nitrate solution is used as the solution containing lead ions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1120452A JPH0637309B2 (en) | 1989-05-16 | 1989-05-16 | Method for producing lead ruthenate fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1120452A JPH0637309B2 (en) | 1989-05-16 | 1989-05-16 | Method for producing lead ruthenate fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02302327A true JPH02302327A (en) | 1990-12-14 |
| JPH0637309B2 JPH0637309B2 (en) | 1994-05-18 |
Family
ID=14786540
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1120452A Expired - Lifetime JPH0637309B2 (en) | 1989-05-16 | 1989-05-16 | Method for producing lead ruthenate fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0637309B2 (en) |
Cited By (3)
| 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 |
| US20120053045A1 (en) * | 2010-08-30 | 2012-03-01 | Jx Nippon Oil & Energy Corporation | Method for preparing pyrochlore-type oxide and method for producing electrocatalyst for fuel cell |
| CN112683611A (en) * | 2020-11-12 | 2021-04-20 | 北京星航机电装备有限公司 | Digestion solution and method for determining element content in refined aluminum ingot for remelting |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3025846U (en) * | 1995-07-11 | 1996-06-25 | 富士男 河合 | A bra that tightens your back with elastics and hook-and-loop fasteners |
-
1989
- 1989-05-16 JP JP1120452A patent/JPH0637309B2/en not_active Expired - Lifetime
Cited By (8)
| 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 |
| US20120053045A1 (en) * | 2010-08-30 | 2012-03-01 | Jx Nippon Oil & Energy Corporation | Method for preparing pyrochlore-type oxide and method for producing electrocatalyst for fuel cell |
| JP2012049075A (en) * | 2010-08-30 | 2012-03-08 | Jx Nippon Oil & Energy Corp | Method of preparing pyrochlore type oxide and method of manufacturing electrode catalyst for fuel cell |
| US8409543B2 (en) * | 2010-08-30 | 2013-04-02 | Jx Nippon Oil & Energy Corporation | Method for preparing pyrochlore-type oxide and method for producing electrocatalyst for fuel cell |
| CN112683611A (en) * | 2020-11-12 | 2021-04-20 | 北京星航机电装备有限公司 | Digestion solution and method for determining element content in refined aluminum ingot for remelting |
| CN112683611B (en) * | 2020-11-12 | 2022-12-06 | 北京星航机电装备有限公司 | Digestion solution and method for determining element content in refined aluminum ingot for remelting |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0637309B2 (en) | 1994-05-18 |
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