JPH051301A - Palladium powder and production thereof - Google Patents
Palladium powder and production thereofInfo
- Publication number
- JPH051301A JPH051301A JP3044327A JP4432791A JPH051301A JP H051301 A JPH051301 A JP H051301A JP 3044327 A JP3044327 A JP 3044327A JP 4432791 A JP4432791 A JP 4432791A JP H051301 A JPH051301 A JP H051301A
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- Japan
- Prior art keywords
- palladium
- solution
- powder
- particle size
- palladium powder
- Prior art date
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Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明はエレクトロニクス用の印
刷、焼成用ペーストの原料として用いられるパラジウム
粉末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 a palladium powder used as a raw material for printing and firing pastes for electronics and a method for producing the same.
【０００２】[0002]
【従来の技術及びその問題点】パラジウム含有ペースト
はパラジウム等の粉末にガラスフリツト、有機ビヒクル
等を混練して得られるものであり、これをセラミツクス
基板等にスクリーン印刷等で塗布し、焼成して電極等の
形成に用いられる。2. Description of the Related Art Palladium-containing paste is obtained by kneading a powder of palladium or the like with glass frit, an organic vehicle or the like. The paste is applied to a ceramic substrate by screen printing or the like and baked to form an electrode. Etc.
【０００３】一般にパラジウム粉末は空気中で焼成する
と昇温過程において５００℃付近から一旦酸化パラジウ
ムを形成し始め、７００℃付近でほぼ完全に酸化物とな
り、さらに８００℃付近で酸素を放出して焼結する。従
つて焼成過程において重量、容量等の変化があるため回
路等の断線、あるいは基板の破損等が生じ易く、基板等
の材質の選定あるいは部品の設計にかなりの制約があつ
た。In general, when a palladium powder is fired in air, it begins to form palladium oxide at about 500 ° C. during the temperature rising process, becomes almost an oxide at about 700 ° C., and releases oxygen at about 800 ° C. to burn. Tie. Therefore, since there are changes in weight, capacity, etc. during the firing process, disconnection of the circuit or the like or breakage of the substrate is likely to occur, and there are considerable restrictions on the selection of the material of the substrate or the design of parts.
【０００４】また、パラジウム粉末の中には、凝集性が
強く単一の粒子に分散せしめるのが困難なものもある。
このような凝集性の強い粒子は、ペーストを作成して塗
布した際に塗布膜の平滑性を損ない、また膜厚を均一に
できないために電気特性の不安定性を生ずる等の問題を
ひきおこしていた。Further, some palladium powders have a strong cohesive property and it is difficult to disperse them into a single particle.
Such particles having a strong cohesive property caused problems such as impairing the smoothness of the coating film when the paste was prepared and applied, and causing instability of electric characteristics because the film thickness could not be made uniform. .
【０００５】[0005]
【発明が解決しようとする問題】本発明の目的は、空気
中での焼成時に室温〜１０００℃までの昇温過程におけ
る重量変化が小さく、しかも凝集傾向が少なく分散性の
良い球状パラジウム粉末、及びその製造方法を提供する
ことにある。DISCLOSURE OF THE INVENTION The object of the present invention is to provide a spherical palladium powder having a small weight change during the temperature rising process from room temperature to 1000 ° C. during firing in air, a small tendency to aggregate, and good dispersibility, and It is to provide the manufacturing method.
【０００６】[0006]
【問題点を解決するための手段】上記目的は、走査型電
子顕微鏡（以下これをＳＥＭという）観察による一次粒
径の分布が０．１〜１μmの範囲の中にあり、レーザー
散乱法による粒度分布の幅が０．１〜１．５μmの範囲
の中にある球状パラジウム粉末において、空気中での焼
成時に室温〜１０００℃までの昇温過程における重量変
化が４重量％以下であることを特徴とする球状パラジウ
ム粉末によつて達成される。[Means for Solving the Problems] The above object is that the distribution of primary particle diameters by observation with a scanning electron microscope (hereinafter referred to as SEM) is in the range of 0.1 to 1 μm, and the particle diameter by laser scattering method is A spherical palladium powder having a distribution width in the range of 0.1 to 1.5 μm, characterized by having a weight change of 4% by weight or less in the temperature rising process from room temperature to 1000 ° C. during firing in air. And spherical palladium powder.
【０００７】また、本発明は、かかる球状パラジウム粉
末の製造方法として、パラジウムアンモニウム錯体溶液
のpHを７〜１１とし、該溶液の温度を５０℃以上に維持
しつつ界面活性剤の存在下で次亜リン酸ナトリウム溶液
を用いて還元することからなる方法を提供する。Further, the present invention provides a method for producing such spherical palladium powder, in which the pH of the palladium ammonium complex solution is set to 7 to 11 and the temperature of the solution is maintained at 50 ° C. or higher in the presence of a surfactant. A method comprising reducing with a sodium phosphite solution is provided.
【０００８】以下本発明について詳細に説明する。The present invention will be described in detail below.
【０００９】本発明のパラジウム粉末は、ＳＥＭ観察に
よつて得られる一次粒径の平均値が０．１〜１μm、好
ましくは０.１〜０.５μm、であり、かつＬＡＳＥＲ散
乱法による粒度分布の範囲が０．１〜１．５μm、好ま
しくは０.１〜１.０μm、の幅に含まれる分散性の良い
粒状粉末であり、さらに空気中にて室温〜１０００℃で
の熱分析におけるＴＧ変化が４重量％以内、好ましくは
３.５％以内、である。The palladium powder of the present invention has an average primary particle size obtained by SEM observation of 0.1 to 1 μm, preferably 0.1 to 0.5 μm, and a particle size distribution by LASER scattering method. Of 0.1 to 1.5 μm, preferably 0.1 to 1.0 μm, is a granular powder having good dispersibility, and TG in thermal analysis at room temperature to 1000 ° C. in air. The change is within 4% by weight, preferably within 3.5%.
【００１０】本発明のパラジウム粉末の製造方法におい
て使用するパラジウムアンモニウム錯体は、例えば硝酸
パラジウム等のパラジウムの酸性溶液をアンモニア水に
て中和したもの、あるいはジクロロジアミンパラジウ
ム、テトラアミンパラジウム溶液等である。反応に使用
するパラジウムアンモニウム錯体のpHは７〜１１の範囲
が望ましい。これはpH７以下ではパラジウムアンモニウ
ム錯体が溶液状態を維持しにくくて沈殿を形成したりす
るためであり、またpH１１以上にするには強アルカリを
多量に混合しなくてはならない事などから実用的でない
ためである。The palladium ammonium complex used in the method for producing the palladium powder of the present invention is, for example, an acidic solution of palladium such as palladium nitrate neutralized with aqueous ammonia, or dichlorodiamine palladium or tetraamine palladium solution. . The pH of the palladium ammonium complex used in the reaction is preferably in the range of 7-11. This is because it is difficult for the palladium ammonium complex to maintain a solution state at pH 7 or lower and forms a precipitate, and at pH 11 or higher, a large amount of strong alkali must be mixed, which is not practical. This is because.
【００１１】反応温度に関しては５０℃以下にすると還
元析出されるパラジウムが反応容器壁に鏡状に析出し易
く、従つて粒子同士の凝集の原因となるため５０℃以上
で反応させる事が望ましい。なお沸騰状態に近くても特
に問題はないが、反応時の取り扱い等を考慮するならば
６０〜９０℃程度が好ましい。反応液に混合する界面活
性剤はアラビアゴム、ゼラチン等様々なものが使用でき
るが、入手方法、安定性、価格等を考慮するならばゼラ
チンが好ましい。なおゼラチンの使用量を少なめにすれ
ば比較的大きな粒子が得られ、また多めにすれば小さめ
の粒子が得られる。従つてゼラチンの使用量を変える事
によつてパラジウム粉末の粒径を変化させる事もでき
る。Regarding the reaction temperature, if the reaction temperature is 50 ° C. or lower, the palladium that is reduced and precipitated is likely to mirror-precipitate on the wall of the reaction vessel, and as a result, it causes agglomeration of particles. It should be noted that there is no particular problem even if it is close to the boiling state, but in consideration of handling during the reaction and the like, about 60 to 90 ° C is preferable. Various surfactants such as gum arabic and gelatin can be used as the surfactant to be mixed with the reaction solution, but gelatin is preferred in view of availability, stability, cost and the like. When the amount of gelatin used is small, relatively large particles can be obtained, and when it is large, small particles can be obtained. Therefore, the particle size of the palladium powder can be changed by changing the amount of gelatin used.
【００１２】還元剤としては次亜リン酸ナトリウムの他
に水素化ホウ素ナトリウム、ジメチルアミンボラン、硫
酸ヒドラジン、塩酸ヒドラジン、ギ酸ナトリウム等につ
いても検討を行つたが、次亜リン酸ナトリウム以外には
目的のパラジウム粉末を得る事はできなかつた。還元剤
の量は反応当量に対して１０〜１５０％多く使用する。
これは反応当量と等量では反応が終了しない場合がある
ために、最低でも１０％余分に使用するのが望ましく、
また反応中に分解される可能性があるため１５０％程度
多く使用する場合もある。還元剤の水溶液の濃度は余り
濃厚になつたりあるいは稀薄にならない方が良く、実用
的には５〜３０％程度が良い。As the reducing agents, sodium hypophosphite, sodium borohydride, dimethylamine borane, hydrazine sulfate, hydrazine hydrochloride, sodium formate, etc. were also investigated, but the objectives other than sodium hypophosphite were investigated. No palladium powder could be obtained. The amount of reducing agent used is 10 to 150% higher than the reaction equivalent.
This is because the reaction may not be completed in the same amount as the reaction equivalent, so it is desirable to use at least 10% extra,
Further, since it may be decomposed during the reaction, it may be used in an amount of about 150%. The concentration of the aqueous solution of the reducing agent should not be too rich or dilute, and is practically about 5 to 30%.
【００１３】反応液の混合速度は速い場合とゆつくりの
場合とで一次粒子の粒度分布に若干の違いを与える。例
えばパラジウムとして１００ｇ以下の小さいスケールで
の反応において反応液の混合速度を３００ｇ Pd／h程度
まで速くすると一次粒子の大きさが揃いにくいが、パラ
ジウムとして１kg以上のスケールにおいては１kg Pd／h
程度まで速くしても粒度分布に特に大きな問題はなかつ
た。従つて反応のスケールと混合速度のバランスを取る
事が重要である。また反応液の添加方法に関しても還元
剤溶液中にパラジウム溶液と添加する方法、パラジウム
溶液中に還元剤溶液を添加する方法等が一般に考えられ
るが、好ましくはパラジウム溶液と還元剤溶液を温水等
を含有する反応槽中に同時に添加し混合する方法が好ま
しい。これは還元剤とパラジウム溶液の濃度を一定にす
るためである。The mixing speed of the reaction solution gives a slight difference in the particle size distribution of the primary particles depending on whether the mixing speed is high or slow. For example, in a reaction on a small scale of 100 g or less as palladium, if the mixing rate of the reaction solution is increased to about 300 g Pd / h, it is difficult to make the primary particles uniform in size, but on a scale of 1 kg or more as palladium, 1 kg Pd / h
Even if the speed was increased to a certain degree, there was no particular problem with the particle size distribution. Therefore, it is important to balance the reaction scale with the mixing rate. Also regarding the method of adding the reaction solution, a method of adding a palladium solution in a reducing agent solution, a method of adding a reducing agent solution in a palladium solution, etc. are generally considered, but preferably the palladium solution and the reducing agent solution are warm water or the like. A method of simultaneously adding and mixing in the contained reaction vessel is preferable. This is to keep the concentrations of the reducing agent and the palladium solution constant.
【００１４】反応の始まりと終りとでpHに大きな差があ
ると一次粒径がそろいにくくなるので、このような場合
には緩衝液等を用いて反応中のpHを常に一定に保つよう
にすることもできる。例えばpH８〜９付近で反応を行な
う場合は緩衝液として酢酸ナトリウム水溶液等を用いる
のが好ましい。If there is a large difference in pH between the beginning and the end of the reaction, it becomes difficult to make the primary particle size uniform. In such a case, use a buffer or the like to keep the pH constant during the reaction. You can also For example, when the reaction is performed at a pH of around 8 to 9, it is preferable to use an aqueous solution of sodium acetate or the like as the buffer solution.
【００１５】[0015]
【実施例】以下本発明の実施例について説明する。EXAMPLES Examples of the present invention will be described below.
【００１６】[0016]
【実施例１】パラジウム硝酸溶液（Ｐｄ１５重量％）２
６７ｇにアンモニア水を加えてpH８に調整し、ゼラチン
０．２ｇをこれに溶解してから液量を６００mlにした。
また次亜リン酸ナトリウム４０ｇを水に溶解し、ゼラチ
ン０．２ｇをこれに溶解してから液量を６００mlにし
た。別にゼラチン０．４ｇを溶解した水１リツトルを用
意し、７０〜７５℃に加熱撹拌しながらここへ上記パラ
ジウム溶液及び次亜リン酸ナトリウム溶液を定量ポンプ
を用いて１．５時間で同時に添加した。反応後約３０分
加熱を続けた後、生成した粉末を洗浄、乾燥した。得ら
れたパラジウム粉末の特性は以下の様な物であつた。Example 1 Palladium nitric acid solution (Pd 15% by weight) 2
Ammonia water was added to 67 g to adjust the pH to 8, 0.2 g of gelatin was dissolved in the solution, and the volume was adjusted to 600 ml.
Further, 40 g of sodium hypophosphite was dissolved in water, 0.2 g of gelatin was dissolved therein, and the liquid volume was adjusted to 600 ml. Separately, 1 liter of water in which 0.4 g of gelatin was dissolved was prepared, and the above palladium solution and sodium hypophosphite solution were simultaneously added thereto while heating and stirring at 70 to 75 ° C. for 1.5 hours using a metering pump. . After continuing the reaction for about 30 minutes, the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００１７】粒形 球状で分散している
一次粒径の分布 ０．２〜０．３μm（ＳＥＭ観察）
粒度分布 ０．１〜０．８μm（レーザー散乱
法）
更に、得られたパラジウム粉末を熱天秤により熱分析
し、図１に示すＴＧ曲線を得た。このＴＧ曲線から重量
変化率が２．２％であることが分る。Grain shape Distribution of spherically dispersed primary particle diameter 0.2 to 0.3 μm (SEM observation) Particle size distribution 0.1 to 0.8 μm (laser scattering method) Further, the obtained palladium powder is heated. Thermal analysis was performed using a balance, and the TG curve shown in FIG. 1 was obtained. From this TG curve, it can be seen that the weight change rate is 2.2%.
【００１８】[0018]
【実施例２】パラジウム硝酸溶液（Ｐｄ１５重量％）２
６７ｇにアンモニア水を加えてpH８に調整し、ゼラチン
０．３ｇをこれに溶解してから液量を６００mlにした。
また次亜リン酸ナトリウム４０ｇを水に溶解し、ゼラチ
ン０．３ｇをこれに溶解してから液量を６００mlにし
た。別にゼラチン０．６ｇを溶解した水１リツトルを用
意し、７０〜７５℃に加熱撹拌しながらここへ上記パラ
ジウム溶液及び次亜リン酸ナトリウム溶液を定量ポンプ
を用いて１．５時間で同時に添加した。反応後約３０分
加熱を続けた後、生成した粉末を洗浄、乾燥した。得ら
れたパラジウム粉末の特性は以下の様な物であつた。Example 2 Palladium nitric acid solution (Pd 15% by weight) 2
Ammonia water was added to 67 g to adjust the pH to 8, and 0.3 g of gelatin was dissolved in this to make the liquid volume 600 ml.
Further, 40 g of sodium hypophosphite was dissolved in water, 0.3 g of gelatin was dissolved therein, and the liquid volume was adjusted to 600 ml. Separately, 1 liter of water in which 0.6 g of gelatin was dissolved was prepared, and the above palladium solution and sodium hypophosphite solution were simultaneously added thereto in 1.5 hours using a metering pump while heating and stirring at 70 to 75 ° C. . After continuing the reaction for about 30 minutes, the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００１９】粒形 球状で分散してい
る
一次粒径の分布 ０．１〜０．３μm（ＳＥＭ観
察）
粒度分布 ０．１〜０．７μm（レーザー
散乱法）
ＴＧ曲線重量変化率 ２．５％Grain shape Distribution of spherically dispersed primary particle diameters 0.1 to 0.3 μm (SEM observation) Particle size distribution 0.1 to 0.7 μm (laser scattering method) TG curve Weight change rate 2.5%
【００２０】[0020]
【実施例３】ジクロロジアミンパラジウム（Ｐｄ５０
％）８０ｇをアンモニア水に溶解してpHを１０にし、ゼ
ラチン０．２ｇを溶解してから液量を６００mlにした。
また次亜リン酸ナトリウム４０ｇを水に溶解し、ゼラチ
ン０．２ｇをこれに溶解してから液量を６００mlにし
た。別にゼラチン０．４ｇを溶解した酢酸ナトリウム水
溶液（５０ｇ／ｌ）１リツトルを用意し、７０〜７５℃
に加熱撹拌しながらここへ上記パラジウム溶液及び次亜
リン酸ナトリウム溶液を定量ポンプに用いて１．５時間
で同時に添加した。反応後約３０分加熱を続けた後、生
成した粉末を洗浄、乾燥した。得られたパラジウム粉末
の特性は以下の様な物であつた。Example 3 Dichlorodiamine palladium (Pd50
%) 80 g was dissolved in aqueous ammonia to adjust the pH to 10, 0.2 g of gelatin was dissolved, and then the liquid volume was adjusted to 600 ml.
Further, 40 g of sodium hypophosphite was dissolved in water, 0.2 g of gelatin was dissolved therein, and the liquid volume was adjusted to 600 ml. Separately, prepare 1 liter of sodium acetate aqueous solution (50 g / l) in which 0.4 g of gelatin is dissolved, and 70-75 ° C
The above-mentioned palladium solution and sodium hypophosphite solution were simultaneously added to the mixture while heating and stirring for 1.5 hours using a metering pump. After continuing the reaction for about 30 minutes, the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００２１】粒形 球状で分散してい
る
一次粒径の分布 ０．２〜０．４μm（ＳＥＭ観
察）
粒度分布 ０．１〜１．０μm（レーザー
散乱法）
ＴＧ曲線重量変化率 ３．５％Grain shape Distribution of spherically dispersed primary particle diameter 0.2 to 0.4 μm (SEM observation) Particle size distribution 0.1 to 1.0 μm (laser scattering method) TG curve Weight change rate 3.5%
【００２２】[0022]
【比較例１】ジクロロジアミンパラジウム（Ｐｄ５０
％）８０ｇを水４リツトルに懸濁させ、塩酸を加えてpH
を１．５に調整し、７０℃に加熱撹拌しながらギ酸ナト
リウム溶液（ギ酸ナトリウム５６ｇを水３００mlに溶解
したもの）を４０分で添加して還元し、反応後約３０分
加熱を続けた後、生成した粉末を洗浄、乾燥した。得ら
れたパラジウム粉末の特性は以下の様な物であつた。Comparative Example 1 Dichlorodiamine palladium (Pd50
%) 80g suspended in 4 liters of water, hydrochloric acid added to pH
Was adjusted to 1.5, a sodium formate solution (56 g of sodium formate dissolved in 300 ml of water) was added for 40 minutes while heating and stirring at 70 ° C. for reduction, and after heating, the heating was continued for about 30 minutes. The produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００２３】粒形 不定形で凝集して
いる
一次粒径の分布 ０．５〜２μm（ＳＥＭ観察）
粒度分布 ０．１〜５μm（レーザー散乱
法）
ＴＧ曲線重量変化率 １５％Grain shape Distribution of primary particle size which is agglomerated in irregular shape 0.5 to 2 μm (SEM observation) Particle size distribution 0.1 to 5 μm (laser scattering method) TG curve Weight change rate 15%
【００２４】[0024]
【比較例２】塩化パラジウム（Ｐｄ５９．４％）６７．
６ｇを塩酸５０リツトルを含んだ水に加熱溶解し、水を
加えて２リツトルとした。水酸化ナトリウム水溶液（Ｎ
ａＯＨ９０ｇを含む）を用いてこれを中和し液量を５リ
ツトルに調整した。これを７０℃に加熱撹拌しながらギ
酸ナトリウム溶液（ギ酸ナトリウム５６ｇを水３００ml
に溶解したもの）を４０分で添加して還元し、反応後約
３０分加熱を続けた後、生成した粉末を洗浄、乾燥し
た。得られたパラジウム粉末の特性は以下の様な物であ
つた。熱分析によるＴＧ曲線を図２に示す。Comparative Example 2 Palladium chloride (Pd 59.4%) 67.
6 g was dissolved by heating in water containing 50 liters of hydrochloric acid, and water was added to make 2 liters. Aqueous sodium hydroxide solution (N
This was neutralized using 90 g of aOH) and the liquid amount was adjusted to 5 liters. A sodium formate solution (56 g of sodium formate was added to 300 ml of water while stirring at 70 ° C).
Was added in 40 minutes for reduction, heating was continued for about 30 minutes after the reaction, and the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows. A TG curve obtained by thermal analysis is shown in FIG.
【００２５】粒形 樹脂状で凝集して
いる
一次粒径の分布 ２０〜３０nm（ＴＥＭ観察）
粒度分布 ０．１〜１．５μm（レーザー
散乱法）
ＴＧ曲線重量変化率 １５％
なお、ＴＥＭ観察とは透過型電子顕微鏡による観察を意
味する。Grain shape Resin-like aggregated primary particle size distribution 20 to 30 nm (TEM observation) Particle size distribution 0.1 to 1.5 μm (laser scattering method) TG curve weight change rate 15% In addition, TEM observation Means observation with a transmission electron microscope.
【００２６】[0026]
【比較例３】パラジウム硝酸溶液（Ｐｄ１５重量％）２
６７ｇにアンモニア水を加えてpH８に調整し、ゼラチン
０．２ｇをこれに溶解してから液量を６００mlにした。
また硫酸ヒドラジン３０ｇを水に溶解し、ゼラチン０．
２ｇをこれに溶解してから液量を６００mlにした。別に
ゼラチン０．４ｇを溶解した酢酸ナトリウム水溶液（５
０ｇ／ｌ）１リツトルを用意し、７０〜７５℃に加熱撹
拌しながらここへ上記パラジウム溶液及び硫酸ヒドラジ
ン溶液を定量ポンプを用いて同時に添加した。反応後約
３０分加熱を続けた後、生成した粉末を洗浄、乾燥し
た。得られたパラジウム粉末の特性は以下の様な物であ
つた。[Comparative Example 3] Palladium nitric acid solution (Pd 15% by weight) 2
Ammonia water was added to 67 g to adjust the pH to 8, 0.2 g of gelatin was dissolved in the solution, and the volume was adjusted to 600 ml.
Also, 30 g of hydrazine sulfate was dissolved in water to prepare gelatin.
2 g was dissolved in this, and the volume was adjusted to 600 ml. Separately, 0.4 g of gelatin was dissolved in an aqueous solution of sodium acetate (5
0 g / l) 1 liter was prepared, and the above palladium solution and hydrazine sulfate solution were simultaneously added thereto while heating and stirring at 70 to 75 ° C using a metering pump. After continuing the reaction for about 30 minutes, the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００２７】粒形 不定形で凝集してい
る（鏡状の物も含まれる）
一次粒径の分布 ０．１〜０．３μm（ＳＥＭ観
察）
（鏡状の物は１０μm以上）
粒度分布 ０．１〜２０μm（レーザー散乱
法）
ＴＧ曲線重量変化率 １５％Grain shape Amorphous aggregates (including mirror-like particles) Primary particle size distribution 0.1 to 0.3 μm (SEM observation) (Mirror-like particles are 10 μm or more) Particle size distribution 0. 1 to 20 μm (laser scattering method) TG curve weight change rate 15%
【００２８】[0028]
【比較例４】パラジウム硝酸溶液（Ｐｄ１５重量％）２
６７ｇにアンモニア水を加えてpH８に調整し、ゼラチン
０．２ｇをこれに溶解してから液量を６００mlにした。
また水酸化ホウ素ナトリウム８ｇを水に溶解し、ゼラチ
ン０．２ｇをこれに溶解してから液量を６００mlにし
た。別にゼラチン０．４ｇを溶解した酢酸ナトリウム水
溶液（５０ｇ／ｌ）１リツトルを用意し、７０〜７５℃
に加熱撹拌しながらここへ上記パラジウム溶液及び水素
化ホウ素ナトリウムを定量ポンプを用いて同時に添加し
た。反応後約３０分加熱を続けた後、生成した粉末を洗
浄、乾燥した。得られたパラジウム粉末の特性は以下の
様な物であつた。Comparative Example 4 Palladium nitric acid solution (Pd 15% by weight) 2
Ammonia water was added to 67 g to adjust the pH to 8, 0.2 g of gelatin was dissolved in the solution, and the volume was adjusted to 600 ml.
Further, 8 g of sodium borohydride was dissolved in water, 0.2 g of gelatin was dissolved therein, and the liquid volume was adjusted to 600 ml. Separately, prepare 1 liter of sodium acetate aqueous solution (50 g / l) in which 0.4 g of gelatin is dissolved, and 70-75 ° C
The above palladium solution and sodium borohydride were simultaneously added to the above while stirring with heating using a metering pump. After continuing the reaction for about 30 minutes, the produced powder was washed and dried. The characteristics of the obtained palladium powder were as follows.
【００２９】粒形 ほとんど凝集して
いる
一次粒径の分布 よく判らない（ＳＥＭ観察）
粒度分布 ０．５〜２５μm（レーザー散
乱法）
ＴＧ曲線重量変化率 １５％Grain shape Almost agglomerated primary particle size distribution Not clear (SEM observation) Particle size distribution 0.5 to 25 μm (laser scattering method) TG curve Weight change rate 15%
【００３０】[0030]
【発明の効果】以上述べたように、本発明のパラジウム
粉末は、平均粒径及び粒度分布の幅が共に小さく、また
昇温過程における重量変化が少なく、更に分散性の良好
な球状粉末である。従つてこれを用いてペーストを作製
し、印刷、焼成することによつてエレクトロニクス用の
電極、回路等を製造する時は、焼成過程における重量変
化が少ないために回路等の断線や基板の破損が大幅に防
止され、また粒子の凝集性が少ないために印刷回路等の
膜厚が一定で平滑になり、従つて電気特性も安定する。As described above, the palladium powder of the present invention is a spherical powder having a small average particle size and a small particle size distribution width, a small weight change in the temperature rising process, and a good dispersibility. . Therefore, when manufacturing electrodes, circuits, etc. for electronics by making paste by using this, printing, and baking, there is little change in weight during the baking process, so disconnection of circuits, etc. It is largely prevented, and since the cohesiveness of the particles is small, the film thickness of the printed circuit is constant and smooth, and the electrical characteristics are stable.
【００３１】また、上記のような優れた特性を有するパ
ラジウム粉末は、本発明の製造方法によつて経済的に効
率良く製造することができる。Further, the palladium powder having the above excellent properties can be economically and efficiently produced by the production method of the present invention.
【図１】実施例１で得られたパラジウム粉末のＴＧ曲線
を示すグラフである。FIG. 1 is a graph showing a TG curve of a palladium powder obtained in Example 1.
【図２】比較例２で得られたパラジウム粉末のＴＧ曲線
の示すグラフである。FIG. 2 is a graph showing a TG curve of a palladium powder obtained in Comparative Example 2.
Claims (2)
１〜１μmの範囲の中にあり、レーザー散乱法による粒
度分布の幅が０．１〜１．５μmの範囲の中にある球状
パラジウム粉末において、空気中での焼成時に室温〜１
０００℃までの昇温過程における重量変化が４重量％以
内であることを特徴とする球状パラジウム粉末。1. The distribution of primary particle diameters by SEM observation is 0.
A spherical palladium powder having a particle size distribution in the range of 1 to 1 μm and a width of particle size distribution measured by a laser scattering method of 0.1 to 1.5 μm is used.
A spherical palladium powder, characterized in that the weight change in the temperature rising process up to 000 ° C is within 4% by weight.
７〜１１とし、該溶液の温度を５０℃以上に維持しつつ
界面活性剤の存在下で次亜リン酸ナトリウム溶液を用い
て還元することを特徴とする請求項１記載のパラジウム
粉末の製造方法。2. A palladium ammonium complex solution having a pH of 7 to 11 and being reduced with a sodium hypophosphite solution in the presence of a surfactant while maintaining the temperature of the solution at 50 ° C. or higher. The method for producing palladium powder according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03044327A JP3122148B2 (en) | 1991-02-16 | 1991-02-16 | Method for producing palladium powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03044327A JP3122148B2 (en) | 1991-02-16 | 1991-02-16 | Method for producing palladium powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH051301A true JPH051301A (en) | 1993-01-08 |
| JP3122148B2 JP3122148B2 (en) | 2001-01-09 |
Family
ID=12688410
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03044327A Expired - Fee Related JP3122148B2 (en) | 1991-02-16 | 1991-02-16 | Method for producing palladium powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3122148B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9020505B2 (en) | 2008-09-17 | 2015-04-28 | Qualcomm Incorporated | Quick system selection and acquisition for multi-mode mobile devices |
-
1991
- 1991-02-16 JP JP03044327A patent/JP3122148B2/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US9020505B2 (en) | 2008-09-17 | 2015-04-28 | Qualcomm Incorporated | Quick system selection and acquisition for multi-mode mobile devices |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3122148B2 (en) | 2001-01-09 |
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