JP2003049202A - Silver particle, manufacturing method thereof and conductive paste - Google Patents
Silver particle, manufacturing method thereof and conductive pasteInfo
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- JP2003049202A JP2003049202A JP2001241505A JP2001241505A JP2003049202A JP 2003049202 A JP2003049202 A JP 2003049202A JP 2001241505 A JP2001241505 A JP 2001241505A JP 2001241505 A JP2001241505 A JP 2001241505A JP 2003049202 A JP2003049202 A JP 2003049202A
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- silver
- silver particles
- aqueous solution
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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- Manufacturing Of Printed Wiring (AREA)
- Conductive Materials (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、銀粒子とその製造
方法、さらにその銀粒子を用いた導電回路形成用導体ペ
ーストに関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to silver particles, a method for producing the same, and a conductive paste for forming a conductive circuit using the silver particles.
【０００２】[0002]
【従来の技術】携帯電話に代表される高密度実装基板、
鉛フリー半田に対応するために高温で焼成する基板な
ど、商品サイクルや技術開発のスピードが速まっている
が、新規な基板に対して適切な導体を用いることで、開
発期間の短縮を計ることができる。これに対応するため
には、粉体物性(粒径、結晶性等)、ペースト特性、その
他に関する様々な特性を有する導体が提供される必要が
ある。これに関連して、低温焼成などに用いる結晶性の
低い銀粒子については、本出願人から多数が提供されて
いる。2. Description of the Related Art A high-density mounting board represented by a mobile phone,
Product cycles and technological development are accelerating, such as substrates that are baked at high temperatures to support lead-free solder, but the development period can be shortened by using appropriate conductors for new substrates. You can In order to deal with this, it is necessary to provide a conductor having various properties regarding powder physical properties (particle size, crystallinity, etc.), paste properties, and the like. In this regard, the present applicant has provided a large number of silver particles having low crystallinity used for low temperature firing and the like.
【０００３】一方で、高温焼成に適する結晶性の高い銀
粒子については、特開２０００―１７０６及び特開２０
００―１７０７が挙げられる。これらは、硝酸銀水溶液
とＬアスコルビン酸水溶液との反応により銀粒子を製造
するものであり、導体ペースト焼成の際の導体とセラミ
ックス基板との収縮差やクラック、デラミネーションの
防止等の効果があると記載されている。On the other hand, silver particles with high crystallinity suitable for high temperature firing are disclosed in JP-A 2000-1706 and JP-A 20-207.
00-1707 can be mentioned. These are for producing silver particles by the reaction of an aqueous solution of silver nitrate and an aqueous solution of L-ascorbic acid, and are effective in preventing shrinkage difference between a conductor and a ceramic substrate during firing of a conductor paste, cracks, delamination, and the like. Have been described.
【０００４】[0004]
【発明が解決しようとする課題】しかしながら、上記の
方法において製造された銀粒子については導体ペースト
の原料としての分散性や流動性の向上がさらに求められ
ていた。However, the silver particles produced by the above method have been further required to have improved dispersibility and fluidity as raw materials for the conductor paste.
【０００５】[0005]
【課題を解決するための手段】本発明者らは導体ペース
トの導体として焼成の際のセラミックス基板との収縮差
の低減のほかに、導体ペーストの粘性低減の観点から特
に表面平滑性およびタップ密度の向上に重点をおいて鋭
意研究した結果、導体ペースト用として好適な銀粒子を
提供するに至った。In order to reduce the difference in shrinkage between the conductor paste and the ceramic substrate during firing as a conductor of the conductor paste, the inventors of the present invention are particularly concerned with surface smoothness and tap density from the viewpoint of reducing the viscosity of the conductor paste. As a result of earnest research focusing on the improvement, it has been possible to provide silver particles suitable for a conductor paste.
【０００６】すなわち、本発明は第１に、結晶子径が４
００〜６００Åであり、タップ密度が５ ｇ／ｃｍ３以
上であることを特徴とする銀粒子；第２に、結晶子径が
４００〜６００Åであり、比表面積が０．１５ ｍ２／
ｇ以下であることを特徴とする銀粒子；第３に、結晶子
径が４００〜６００Åであり、タップ密度が５ ｇ／ｃ
ｍ３以上であり、比表面積が０．１５ ｍ２／ｇ以下で
あることを特徴とする銀粒子；第４に、前記銀粒子が導
体ペーストの導体用銀粒子である、第１〜３のいずれか
に記載の銀粒子；第５に、銀イオンを含有するアルカリ
性水溶液と過酸化水素水溶液とを反応させることを特徴
とする、第１〜４のいずれかに記載の銀粒子の製造方
法；第６に、前記反応に際し、脂肪酸、脂肪酸塩および
それらの誘導体からなる群から選ばれる１種以上を存在
させる、第５記載の製造方法；第７に、前記アルカリ性
水溶液が水酸化アンモニウム水溶液であり、前記反応に
際し水酸化ナトリウムおよび水酸化カリウムからなる群
から選ばれる１種以上が添加される、第５または６記載
の製造方法；第８に、前記脂肪酸がステアリン酸および
オレイン酸からなる群から選ばれる１種以上であり、前
記脂肪酸塩がステアリン酸ナトリウムおよびオレイン酸
ナトリウムからなる群から選ばれる１種以上である、第
６または７記載の製造方法；第９に、前記の脂肪酸、脂
肪酸塩およびそれらの誘導体からなる群から選ばれる１
種以上の添加量が前記アルカリ性水溶液中の銀イオンの
重量の０．００１〜０．５％である、第６〜８のいずれ
かに記載の製造方法；第１０に、第１〜３のいずれかに
記載の銀粒子を導体に用いたことを特徴とする、導体ペ
ースト、を提供するものである。That is, first, the present invention has a crystallite diameter of 4
0 to 600Å and a tap density of 5 g / cm 3 or more; secondly, a crystallite diameter of 400 to 600Å and a specific surface area of 0.15 m 2 /
Silver particles characterized by being less than or equal to g; Thirdly, the crystallite diameter is 400 to 600Å, and the tap density is 5 g / c.
m 3 or more and a specific surface area of 0.15 m 2 / g or less; silver particles; fourth, the silver particles are conductor silver particles of a conductor paste; Silver particles according to any one of the above; fifth, the method for producing silver particles according to any one of the first to fourth, characterized by reacting an alkaline aqueous solution containing silver ions with an aqueous hydrogen peroxide solution; Sixth, in the reaction, at least one selected from the group consisting of fatty acids, fatty acid salts and their derivatives is present, and seventh, the alkaline aqueous solution is an aqueous ammonium hydroxide solution. The method according to the fifth or sixth aspect, wherein at least one selected from the group consisting of sodium hydroxide and potassium hydroxide is added during the reaction; eighth, the fatty acid comprises stearic acid and oleic acid. At least one selected from the group, wherein the fatty acid salt is at least one selected from the group consisting of sodium stearate and sodium oleate; ninth, the production method according to the seventh; 1 selected from the group consisting of fatty acid salts and their derivatives
The manufacturing method according to any one of 6th to 8th, wherein the addition amount of at least one species is 0.001 to 0.5% of the weight of silver ions in the alkaline aqueous solution; The present invention provides a conductor paste, characterized in that the silver particles described in (1) are used for a conductor.
【０００７】[0007]
【発明の実施の形態】本発明における銀粒子の結晶子径
は、次のScherrerの式によって求められる。すなわち、
Ｄhkl＝Ｋλ／βcosθ
ここで、
Ｄhkl（Å）：結晶子径の大きさ（hklに垂直な方向の結
晶子の大きさ）
λ（Å）：測定Ｘ線の波長（Ｃｕターゲット使用時１．
５４０５Å）
β（rad）：結晶子の大きさによる回折線の広がりであ
り、半価幅を用いる。
θ（rad）：回折線のブラッグ角であって、入射角と反
射角が等しいときの角度であり、ピークトップの角度を
使用する。
Ｋ：Scherrer定数（Ｄやβの定義により異なる。βに半
価幅を用いる場合Ｋ＝０．９４）
なお、測定は粉末Ｘ線回折装置を用い、計算には（２０
０）面のピークデータを用いる。BEST MODE FOR CARRYING OUT THE INVENTION The crystallite size of silver particles in the present invention is determined by the following Scherrer's equation. That is, D hkl = Kλ / β cos θ, where D hkl (Å): size of crystallite size (size of crystallite in the direction perpendicular to hkl) λ (Å): wavelength of measured X-ray (using Cu target) When 1.
5405 Å) β (rad): spread of diffraction line due to size of crystallite, half width is used. θ (rad): Bragg angle of the diffraction line, which is the angle when the incident angle and the reflection angle are equal, and the peak top angle is used. K: Scherrer constant (varies depending on the definition of D and β. K = 0.94 when half-value width is used for β) Note that the measurement was performed using a powder X-ray diffractometer, and the calculation was performed using (20
The peak data of the 0) plane is used.
【０００８】また、本発明においては比表面積（ｍ２／
g）の値はＢＥＴ法で求める。銀粒子の結晶子径の範囲
は４００〜６００Åであり、好ましくは４００〜５００
Åである。４００Å未満では高温焼成導体ペースト用の
銀粒子としては結晶性が低く、６００Åを超えると銀粒
子形状が不安定化し、導体ペーストの粘性が増加する。
銀粒子のタップ密度については５ｇ／ｃｍ３以上であ
る。銀粒子のタップ密度が５ｇ／ｃｍ３未満では導体ペ
ーストを焼成後の導電回路の緻密性および表面平滑性が
損なわれ高密度実装基板用に適用困難である。また、銀
粒子の比表面積については０．１５ｍ２／g以下であ
る。銀粒子の比表面積が０．１５ｍ２／gを超えると表
面平滑性が損なわれる。In the present invention, the specific surface area (m 2 /
The value of g) is calculated by the BET method. The crystallite size of the silver particles is 400 to 600Å, preferably 400 to 500.
It is Å. If it is less than 400 Å, the crystallinity is low as silver particles for high temperature firing conductor paste, and if it exceeds 600 Å, the shape of silver particles becomes unstable and the viscosity of the conductor paste increases.
The tap density of silver particles is 5 g / cm 3 or more. If the tap density of the silver particles is less than 5 g / cm 3 , the denseness and surface smoothness of the conductive circuit after firing the conductor paste will be impaired and it will be difficult to apply it to a high-density mounting substrate. The specific surface area of the silver particles is 0.15 m 2 / g or less. If the specific surface area of the silver particles exceeds 0.15 m 2 / g, the surface smoothness will be impaired.
【０００９】銀粒子の製造にあたっては、銀イオンを含
有するアルカリ性水溶液を過酸化水素水溶液と反応させ
て還元し銀粒子を析出させるが、銀イオン源としては硝
酸銀が好ましい。実施例で詳細に記載するがここで銀粒
子の製造方法をより具体的に記載すると、ビーカーに純
水を入れ、５０℃に液温を調節した後、硝酸銀水溶液
と、水酸化アンモニウム水溶液（アンモニア水溶液とい
うことがある。）を添加する。５０℃を維持したまま、
銀の錯体が形成されるだけの時間撹拌後、好ましくは硝
酸アンモニウムを添加し、過酸化水素水溶液好ましくは
過酸化水素水溶液と水酸化ナトリウム水溶液および水酸
化カリウムの１種以上をほぼ同時に液中あるいは液表面
に撹拌しながら添加する。過酸化水素水溶液単独で添加
しても目的が達せられるが、銀の還元の途中でｐＨが低
下し、還元反応速度が低下してくるため、水酸化ナトリ
ウム、水酸化カリウム等のアルカリを同時に添加するこ
とでｐＨの低下を防止し銀粒子の収量をより向上させる
ことができる。In the production of silver particles, an alkaline aqueous solution containing silver ions is reacted with an aqueous solution of hydrogen peroxide for reduction to deposit silver particles, and silver nitrate is preferred as the silver ion source. The method for producing silver particles will be described in more detail in the examples, but more specifically, pure water is put in a beaker and the liquid temperature is adjusted to 50 ° C., and then a silver nitrate aqueous solution and an ammonium hydroxide aqueous solution (ammonia It may be referred to as an aqueous solution). While maintaining 50 ℃,
After stirring for a time to form a silver complex, ammonium nitrate is preferably added, and an aqueous solution of hydrogen peroxide, preferably one or more of an aqueous solution of hydrogen peroxide and an aqueous solution of sodium hydroxide and potassium hydroxide, is added to the liquid or liquid at about the same time. Add to surface with stirring. Although the purpose can be achieved by adding the hydrogen peroxide solution alone, the pH decreases during the reduction of silver and the reduction reaction rate decreases, so alkali such as sodium hydroxide and potassium hydroxide is added at the same time. By so doing, it is possible to prevent a decrease in pH and further improve the yield of silver particles.
【００１０】また反応に際し、ステアリン酸やオレイン
酸等の脂肪酸、ステアリン酸ナトリウム（ステアリン酸
ソーダということがある。）やオレイン酸ナトリウム
（オレイン酸ソーダということがある。）等の脂肪酸
塩、またはそれらの誘導体を添加することで分散性の良
い銀粒子を得ることができる。これらの添加量は前記ア
ルカリ性水溶液中の銀イオンの重量の０．００１〜０．
５重量％（単に、％と表す。）とする。添加量が０．０
０１％未満では添加効果が発揮されず、０．５％以上で
は効果が飽和する。また、反応に際しては、その添加時
期も重要であり、過酸化水素水溶液の添加前、添加中、
添加直後、添加後、添加液への混合等いずれでも効果が
あるが、過酸化水素水溶液の添加前、添加直後の添加が
より効果的である。In the reaction, fatty acids such as stearic acid and oleic acid, fatty acid salts such as sodium stearate (sometimes called sodium stearate) and sodium oleate (sometimes called sodium oleate), or those. A silver particle having good dispersibility can be obtained by adding the derivative of. The amount of these added is 0.001 to 0. 0 of the weight of silver ions in the alkaline aqueous solution.
5 wt% (simply expressed as%). Addition amount is 0.0
If it is less than 01%, the effect of addition is not exhibited, and if it is 0.5% or more, the effect is saturated. In addition, in the reaction, the timing of addition is also important.
Immediately after the addition, after the addition, mixing with the addition liquid, etc. are effective, but addition before and immediately after the addition of the aqueous hydrogen peroxide solution is more effective.
【００１１】[0011]
【実施例】以下の実施例によって本発明を説明するが、
本発明はこれら実施例に限定されるものではない。The present invention will be described with reference to the following examples.
The present invention is not limited to these examples.
【００１２】[ 実施例１] １０Ｌのビーカーに純水を
６６００ｇ入れ液温を５０℃に保つ。これに硝酸銀水溶
液（銀７７ｇ相当）、アンモニア水溶液（アンモニア６
７ｇ相当）を撹拌しながら添加し、１５分間撹拌後、硝
酸アンモニウム１０ｇ、ステアリン酸ソーダ水１００ m
l（ステアリン酸ソーダ添加比率：５００ ppm／Ag）を
添加し、その後過酸化水素水溶液（３．３ mol／L）
と、水酸化ナトリウム水溶液（０．８ mol／L）とをそ
れぞれ２００ ml／minの速度で同時に２４０秒間添加す
る。得られた銀粒子の結晶子径、タップ密度および比表
面積は表１のとおりである。Example 1 6600 g of pure water was placed in a 10 L beaker and the liquid temperature was kept at 50 ° C. To this, an aqueous silver nitrate solution (equivalent to 77 g of silver) and an aqueous ammonia solution (ammonia 6
(Equivalent to 7 g) is added with stirring, and after stirring for 15 minutes, ammonium nitrate 10 g, sodium stearate water 100 m
l (sodium stearate addition ratio: 500 ppm / Ag) was added, followed by hydrogen peroxide solution (3.3 mol / L)
And sodium hydroxide aqueous solution (0.8 mol / L) are simultaneously added at a rate of 200 ml / min for 240 seconds. Table 1 shows the crystallite size, tap density and specific surface area of the obtained silver particles.
【００１３】[0013]
【表１】 [Table 1]
【００１４】[ 実施例２] １０Ｌのビーカーに純水を
６６００ｇ入れ液温を５０℃に保つ。これに硝酸銀水溶
液（銀７７ｇ相当）、アンモニア水溶液（アンモニア６
７ｇ相当）を撹拌しながら添加し、１５分間撹拌後、硝
酸アンモニウム１０ｇを添加し、その後過酸化水素水溶
液（３．３ mol／L）と、水酸化ナトリウム水溶液
（０．８ mol／L）をそれぞれ２００ ml／minの速度で
同時に１２０秒間添加し、添加開始２０秒後にオレイン
酸ソーダ水１３６ ml（オレイン酸ソーダ添加比率：５
００ ppm／Ag）を添加する。得られた銀粒子の結晶子
径、タップ密度および比表面積は表１のとおりである。[Example 2] 6600 g of pure water was placed in a 10 L beaker and the liquid temperature was kept at 50 ° C. To this, an aqueous silver nitrate solution (equivalent to 77 g of silver) and an aqueous ammonia solution (ammonia 6
7 g) was added with stirring, and after stirring for 15 minutes, 10 g of ammonium nitrate was added, and then an aqueous hydrogen peroxide solution (3.3 mol / L) and an aqueous sodium hydroxide solution (0.8 mol / L) were respectively added. The mixture was added simultaneously at a rate of 200 ml / min for 120 seconds, and 20 seconds after the start of addition, 136 ml of sodium oleate water (sodium oleate addition ratio: 5
00 ppm / Ag) is added. Table 1 shows the crystallite size, tap density and specific surface area of the obtained silver particles.
【００１５】[ 実施例３] 過酸化水素水溶液と水酸化
ナトリウム水溶液を２４０秒間添加する以外は実施例２
と同一条件で行った。得られた銀粒子の結晶子径、タッ
プ密度および比表面積は表１のとおりである。Example 3 Example 2 except that a hydrogen peroxide aqueous solution and a sodium hydroxide aqueous solution were added for 240 seconds.
The same conditions were used. Table 1 shows the crystallite size, tap density and specific surface area of the obtained silver particles.
【００１６】[ 実施例４] １０Ｌのビーカーに純水を
６６００ｇ入れ液温を５０℃に保つ。これに硝酸銀水溶
液（銀７７ｇ相当）、アンモニア水溶液（アンモニア６
７ｇ相当）を撹拌しながら添加し、１５分間撹拌後、硝
酸アンモニウム１０ｇ、オレイン酸ソーダを８０ml（オ
レイン酸ソーダ添加比率：５００ ppm／Ag）を添加し、
その後過酸化水素水溶液（３．３ mol／L ）と、水酸化
ナトリウム水溶液（１．６ mol／L ）をそれぞれ２００
ml／min の速度で同時に２４０秒間添加し、添加開始
後１０秒後にオレイン酸ソーダ８０ml（オレイン酸ソー
ダ添加比率：５００ppm／Ag）を添加する。得られた銀
粒子の結晶子径、タップ密度および比表面積は表１のと
おりである。Example 4 6600 g of pure water was placed in a 10 L beaker and the liquid temperature was kept at 50 ° C. To this, an aqueous silver nitrate solution (equivalent to 77 g of silver) and an aqueous ammonia solution (ammonia 6
7 g) is added with stirring, and after stirring for 15 minutes, 10 g of ammonium nitrate and 80 ml of sodium oleate (sodium oleate addition ratio: 500 ppm / Ag) are added,
Then, the hydrogen peroxide solution (3.3 mol / L) and the sodium hydroxide solution (1.6 mol / L) were each added to 200 times.
The mixture is added simultaneously at a rate of ml / min for 240 seconds, and 10 seconds after the start of the addition, 80 ml of sodium oleate (sodium oleate addition ratio: 500 ppm / Ag) is added. Table 1 shows the crystallite size, tap density and specific surface area of the obtained silver particles.
【００１７】[ 比較例１] １００mlビーカーに純水約
５０mlを入れ、ここに硝酸銀溶液(銀６g相当)を加え、c
onc.の過酸化水素水溶液１０mlを添加した。その結果、
発泡したが、固体の生成は無く、酸性水溶液中の銀イオ
ンは過酸化水素水溶液によっては還元されなかった。[Comparative Example 1] About 50 ml of pure water was placed in a 100 ml beaker, and a silver nitrate solution (corresponding to 6 g of silver) was added to the beaker.
10 ml of an onc. hydrogen peroxide solution was added. as a result,
Although foaming occurred, no solid was produced and silver ions in the acidic aqueous solution were not reduced by the aqueous hydrogen peroxide solution.
【００１８】[ 比較例２] 銀１０g/Lの硝酸銀溶液に適
量のアンモニア水溶液を加え、銀アンミン錯体水溶液を
作製し、液温を４０℃に保持したまま、撹拌しながら所
定量の３７％濃度のホルマリン水溶液を添加した。得ら
れた銀粒子の結晶子径は２９３Å、タップ密度は３．７
５g/cm3、比表面積は０．２３m2/gであった。[Comparative Example 2] An appropriate amount of an aqueous ammonia solution was added to a silver nitrate solution containing 10 g / L of silver to prepare an aqueous solution of a silver ammine complex. Formalin aqueous solution was added. The obtained silver particles have a crystallite size of 293Å and a tap density of 3.7.
The specific surface area was 5 g / cm 3 and 0.23 m 2 / g.
【００１９】[ 比較例３] １０Ｌのビーカーに純水を
６６００ｇ入れ液温を５０℃に保つ。これに硝酸銀水溶
液（銀７７ｇ相当）、アンモニア水溶液（アンモニア６
７ｇ相当）を撹拌しながら添加し、１５分間撹拌後、硝
酸アンモニウム１２．５ｇを添加し、その後過酸化水素
水溶液（３．３ mol／L ）と、水酸化ナトリウム水溶液
（１．６ mol／L ）をそれぞれ２００ ml／min の速度
で同時に６０秒間添加し、添加開始と同時に別系統で過
酸化水素のconc.溶液５２．５ｇを一度に添加する。得
られた銀粒子の結晶子径は４０５Å、タップ密度は３．
５９g/cm3、比表面積は０．１６m2/gであった。Comparative Example 3 6600 g of pure water was placed in a 10 L beaker and the liquid temperature was kept at 50 ° C. To this, an aqueous silver nitrate solution (equivalent to 77 g of silver) and an aqueous ammonia solution (ammonia 6
7 g) was added with stirring, and after stirring for 15 minutes, 12.5 g of ammonium nitrate was added, and then an aqueous solution of hydrogen peroxide (3.3 mol / L) and an aqueous solution of sodium hydroxide (1.6 mol / L) were added. Are simultaneously added at a rate of 200 ml / min for 60 seconds, and 52.5 g of a conc. Solution of hydrogen peroxide is added at once at the same time when the addition is started. The obtained silver particles had a crystallite size of 405Å and a tap density of 3.
The specific surface area was 59 g / cm 3 and 0.16 m 2 / g.
【００２０】[0020]
【発明の効果】本発明によれば、結晶子径が４００〜６
００Åと結晶性が高く、タップ密度が５ ｇ／ｃｍ３以
上、比表面積が０．１５ ｍ２／ｇ以下の銀粒子を効率
的に製造することができる。また、これらの銀粒子を用
いた導体ペーストは高温焼成用に最適であり、ペースト
粘性が低減されて印刷性に優れ、さらに焼成後の回路が
緻密性と表面平滑性とを有するものである。According to the present invention, the crystallite diameter is 400 to 6
It is possible to efficiently produce silver particles having a high crystallinity of 00Å, a tap density of 5 g / cm 3 or more, and a specific surface area of 0.15 m 2 / g or less. Further, the conductor paste using these silver particles is most suitable for high-temperature firing, the paste viscosity is reduced and the printability is excellent, and the circuit after firing has denseness and surface smoothness.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 大内 正美 東京都千代田区丸の内一丁目８番２号 同 和鉱業株式会社内 (72)発明者 上田 俊雄 東京都千代田区丸の内一丁目８番２号 同 和鉱業株式会社内 Ｆターム(参考） 4K017 AA03 BA02 DA01 EJ01 EJ02 FB07 FB11 4K018 BA01 BB04 BB10 BD01 KA33 5E343 BB25 BB72 GG11 5G301 DA03 DD01 ─────────────────────────────────────────────────── ─── Continued front page (72) Masami Ouchi 1-8-2 Marunouchi, Chiyoda-ku, Tokyo Within Wa Mining Co., Ltd. (72) Inventor Toshio Ueda 1-8-2 Marunouchi, Chiyoda-ku, Tokyo Within Wa Mining Co., Ltd. F-term (reference) 4K017 AA03 BA02 DA01 EJ01 EJ02 FB07 FB11 4K018 BA01 BB04 BB10 BD01 KA33 5E343 BB25 BB72 GG11 5G301 DA03 DD01
Claims (10)
ップ密度が５ ｇ／ｃｍ３以上であることを特徴とする
銀粒子。1. Silver particles having a crystallite diameter of 400 to 600 Å and a tap density of 5 g / cm 3 or more.
表面積が０．１５ｍ２／ｇ以下であることを特徴とする
銀粒子。2. A silver particle having a crystallite diameter of 400 to 600Å and a specific surface area of 0.15 m 2 / g or less.
ップ密度が５ ｇ／ｃｍ３以上であり、比表面積が０．
１５ ｍ２／ｇ以下であることを特徴とする銀粒子。3. The crystallite diameter is 400 to 600Å, the tap density is 5 g / cm 3 or more, and the specific surface area is 0.
The silver particles are 15 m 2 / g or less.
子である、請求項１〜３のいずれかに記載の銀粒子。4. The silver particle according to claim 1, wherein the silver particle is a conductor silver particle of a conductor paste.
過酸化水素水溶液とを反応させることを特徴とする、請
求項１〜４のいずれかに記載の銀粒子の製造方法。5. The method for producing silver particles according to claim 1, wherein an alkaline aqueous solution containing silver ions is reacted with an aqueous hydrogen peroxide solution.
びそれらの誘導体からなる群から選ばれる１種以上を存
在させる、請求項５記載の製造方法。6. The production method according to claim 5, wherein one or more kinds selected from the group consisting of fatty acids, fatty acid salts and their derivatives are present in the reaction.
ウム水溶液であり、前記反応に際し水酸化ナトリウムお
よび水酸化カリウムからなる群から選ばれる１種以上が
添加される、請求項５または６記載の製造方法。7. The production method according to claim 5, wherein the alkaline aqueous solution is an ammonium hydroxide aqueous solution, and at least one selected from the group consisting of sodium hydroxide and potassium hydroxide is added during the reaction.
ン酸からなる群から選ばれる１種以上であり、前記脂肪
酸塩がステアリン酸ナトリウムおよびオレイン酸ナトリ
ウムからなる群から選ばれる１種以上である、請求項６
または７記載の製造方法。8. The fatty acid is one or more selected from the group consisting of stearic acid and oleic acid, and the fatty acid salt is one or more selected from the group consisting of sodium stearate and sodium oleate. 6
Or the manufacturing method according to 7.
誘導体からなる群から選ばれる１種以上の添加量が前記
アルカリ性水溶液中の銀イオンの重量の０．００１〜
０．５ ％である、請求項６〜８のいずれかに記載の製
造方法。9. The addition amount of one or more kinds selected from the group consisting of the fatty acids, fatty acid salts and their derivatives is 0.001 to 0.001 of the weight of silver ions in the alkaline aqueous solution.
It is 0.5%, The manufacturing method in any one of Claims 6-8.
子を導体に用いたことを特徴とする、導体ペースト。10. A conductor paste comprising the silver particles according to claim 1 as a conductor.
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| JP2001241505A JP4639395B2 (en) | 2001-08-09 | 2001-08-09 | Method for producing silver particles |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1666174A3 (en) * | 2004-11-25 | 2006-09-13 | Dowa Mining Co., Ltd. | Silver powder and method for producing same |
| JP2007194581A (en) * | 2005-12-21 | 2007-08-02 | E I Du Pont De Nemours & Co | Paste for solar cell electrode |
| JP2007254846A (en) * | 2006-03-24 | 2007-10-04 | Mitsui Mining & Smelting Co Ltd | Production method for copper powder and copper powder obtained by the production method |
| CN102189270A (en) * | 2011-05-04 | 2011-09-21 | 上海大学 | Method for chemically synthesizing nano lead-free solder particles with low melting point |
| JP2013159804A (en) * | 2012-02-02 | 2013-08-19 | Toda Kogyo Corp | Silver microparticle, method for producing same, and conductive paste, conductive film and electronic device containing silver microparticle |
| JP2013159805A (en) * | 2012-02-02 | 2013-08-19 | Toda Kogyo Corp | Method for producing silver microparticle, silver microparticle produced by the method for producing silver microparticle, and conductive paste containing the silver microparticle |
| US8721931B2 (en) | 2005-12-21 | 2014-05-13 | E I Du Pont De Nemours And Company | Paste for solar cell electrode, solar cell electrode manufacturing method, and solar cell |
| WO2017026723A1 (en) * | 2015-08-12 | 2017-02-16 | 엘에스니꼬동제련 주식회사 | Silver powder and preparing method therefor |
| CN107876799A (en) * | 2017-12-18 | 2018-04-06 | 西安宏星电子浆料科技有限责任公司 | High-tap density low specific surface area super fine silver powder and preparation method thereof |
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| KR20180047527A (en) * | 2016-10-31 | 2018-05-10 | 엘에스니꼬동제련 주식회사 | Surface treated silver powder and manufacturing method of the same |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1666174A3 (en) * | 2004-11-25 | 2006-09-13 | Dowa Mining Co., Ltd. | Silver powder and method for producing same |
| KR101141839B1 (en) | 2004-11-25 | 2012-05-07 | 도와 홀딩스 가부시키가이샤 | Silver Powder and Method for Producing Same |
| US8282702B2 (en) | 2004-11-25 | 2012-10-09 | Dowa Mining Co., Ltd. | Silver powder and method for producing same |
| JP2007194581A (en) * | 2005-12-21 | 2007-08-02 | E I Du Pont De Nemours & Co | Paste for solar cell electrode |
| US8721931B2 (en) | 2005-12-21 | 2014-05-13 | E I Du Pont De Nemours And Company | Paste for solar cell electrode, solar cell electrode manufacturing method, and solar cell |
| JP2007254846A (en) * | 2006-03-24 | 2007-10-04 | Mitsui Mining & Smelting Co Ltd | Production method for copper powder and copper powder obtained by the production method |
| CN102189270A (en) * | 2011-05-04 | 2011-09-21 | 上海大学 | Method for chemically synthesizing nano lead-free solder particles with low melting point |
| JP2013159804A (en) * | 2012-02-02 | 2013-08-19 | Toda Kogyo Corp | Silver microparticle, method for producing same, and conductive paste, conductive film and electronic device containing silver microparticle |
| JP2013159805A (en) * | 2012-02-02 | 2013-08-19 | Toda Kogyo Corp | Method for producing silver microparticle, silver microparticle produced by the method for producing silver microparticle, and conductive paste containing the silver microparticle |
| WO2017026723A1 (en) * | 2015-08-12 | 2017-02-16 | 엘에스니꼬동제련 주식회사 | Silver powder and preparing method therefor |
| CN107876799A (en) * | 2017-12-18 | 2018-04-06 | 西安宏星电子浆料科技有限责任公司 | High-tap density low specific surface area super fine silver powder and preparation method thereof |
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