JP2590869B2 - Manufacturing method of plating solution for solder - Google Patents
Manufacturing method of plating solution for solderInfo
- Publication number
- JP2590869B2 JP2590869B2 JP62083673A JP8367387A JP2590869B2 JP 2590869 B2 JP2590869 B2 JP 2590869B2 JP 62083673 A JP62083673 A JP 62083673A JP 8367387 A JP8367387 A JP 8367387A JP 2590869 B2 JP2590869 B2 JP 2590869B2
- Authority
- JP
- Japan
- Prior art keywords
- tin
- lead
- solution
- aromatic
- sulfonic acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
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- Electroplating And Plating Baths Therefor (AREA)
Description
【発明の詳細な説明】 (産業分野) 本発明は通常のICは勿論のこと、大容量メモリー素子
である256K RAM式或はそれ以上のメモリーや各種超LSI
等の半導体装置の部品、基板等にハンダ用合金をメツキ
するのに適した芳香族スルフオン酸及びその鉛塩、錫塩
を含む低α放射能のハンダ用メツキ液に関する。DETAILED DESCRIPTION OF THE INVENTION (Industrial Field) The present invention is not limited to ordinary ICs, but also includes a 256K RAM type memory or larger memory as a large-capacity memory element and various super LSIs.
The present invention relates to a low α-activity solder plating solution containing an aromatic sulfonic acid and a lead salt and a tin salt thereof suitable for plating a solder alloy on a component of a semiconductor device such as a substrate, a substrate, or the like.
(従来技術とその問題点) 従来は鉛及び錫中のα線発生源であるU,Thを多量に含
む化合物を用いて調製したハンダ用メツキ液はメツキ後
にハンダ電着物からα線を多数発生するため、いわゆる
メモリーデバイスのソフトエラーを惹起していた。(Conventional technology and its problems) Conventionally, a solder plating solution prepared using a compound containing a large amount of U and Th, which is a source of α-rays in lead and tin, generates many α-rays from the solder electrodeposit after plating. This causes a so-called soft error in the memory device.
従来技術の一例について述べる。すなわち、従来法に
よつて調製されたハンダ用メツキ液を用いて作成された
ハンダ膜中には、U,Th等の放射性同位元素が100ppb以上
も含有されており、これは放射性α粒子のカウント数と
して数CPH/cm2〜数100CPH/cm2に相当するものである。
このように、予備精製を施さない放射性同位元素の含有
量が高い鉛、錫化合物を主成分とするハンダ用メツキ液
を半導体装置組立に用いると、作成されたハンダ膜から
発する放射性α粒子がメモリーエラーの原因となり、信
頼性の乏しいものとなつていた。An example of the related art will be described. That is, a solder film prepared using a solder plating solution prepared by a conventional method contains radioactive isotopes such as U and Th in an amount of 100 ppb or more. it is equivalent to the number CPH / cm 2 ~ number 100CPH / cm 2 as a number.
As described above, when a solder plating solution mainly containing a lead and tin compound having a high content of radioisotope which is not subjected to pre-purification is used for assembling a semiconductor device, radioactive α particles emitted from the formed solder film are stored in a memory. It caused errors and was unreliable.
本発明者らは、上記の従来技術の問題点を解決し、半
導体装置のメモリーエラーの発生を抑制するハンダ用メ
ツキ液を提供すべく研究を重ねた結果、メツキによつて
形成されたハンダ膜の主成分であるPb,Sn中に不可避不
純物として含まれている放射性同位元素のU,Th量を20pp
b未満とすると、放射性α粒子のカウント数を0.1CPH/cm
2以下に抑制できることを見出し、本発明に到達した。The inventors of the present invention have conducted various studies to solve the above-mentioned problems of the prior art and to provide a solder plating solution for suppressing the occurrence of memory errors in a semiconductor device. As a result, a solder film formed by the plating has been developed. The amount of radioactive isotopes U and Th contained as inevitable impurities in Pb and Sn, which are the main components of
If it is less than b, the count of radioactive α particles is 0.1 CPH / cm
They have found that they can be suppressed to 2 or less, and have reached the present invention.
(発明の構成) 本発明によれば、次の一般式 (式中、R1及びR2は同一又は異なっていてもよく、それ
ぞれ水素原子、水酸基、低級アルキル基及びスルフォン
酸基よりなる群の中から選ばれる)で表わされる芳香族
スルフォン酸ならびに該芳香族スルフォン酸の鉛塩およ
び錫塩を含有するハンダ用メッキ液の製造方法であっ
て、いずれも下記〜の工程により製造された高純度
の前記芳香族スルフォン酸の鉛塩および錫塩を前記芳香
族スルフォン酸に溶解させることを特徴とする、放射性
同位元素の含有量が20ppb未満で、放射性α粒子のカウ
ント数が0.1CPH/cm2未満のハンダ用メッキ液の製造方法
が提供される。(Constitution of the Invention) According to the present invention, the following general formula Wherein R 1 and R 2 may be the same or different and each is selected from the group consisting of a hydrogen atom, a hydroxyl group, a lower alkyl group and a sulfonic acid group, and the aromatic sulfonic acid represented by the formula A method for producing a solder plating solution containing a lead salt and a tin salt of an aromatic sulfonic acid, wherein each of the lead salt and the tin salt of the high-purity aromatic sulfonic acid produced by the following steps (a) to (e) is subjected to the aromatic treatment. A method for producing a solder plating solution characterized by being dissolved in an aromatic sulfonic acid, wherein the content of a radioisotope is less than 20 ppb and the count number of radioactive α particles is less than 0.1 CPH / cm 2 .
純度が99.99%以上の鉛および/または錫を高純度硝
酸水溶液に溶解し、 得られた溶液の遊離硝酸濃度を5〜10モルに調整し、 濃度調整した溶液を陰イオン交換樹脂で精製して、溶
液中のUおよびThの含有量を低減させ、 精製した溶液に芳香族スルフォン酸を反応させた後、
中和して、放射性同位元素の含有量が20ppb未満で、放
射性α粒子のカウント数が0.1CPH/cm2未満である高純度
の芳香族スルフォン酸の鉛塩および/または錫塩を生成
させる。Dissolve lead and / or tin with a purity of 99.99% or more in a high-purity nitric acid aqueous solution, adjust the free nitric acid concentration of the obtained solution to 5 to 10 mol, and purify the concentration-adjusted solution with an anion exchange resin. Reducing the content of U and Th in the solution, and reacting the purified solution with aromatic sulfonic acid,
Neutralization produces a high purity lead and / or tin salt of aromatic sulfonic acid with a radioisotope content of less than 20 ppb and a radioactive α particle count of less than 0.1 CPH / cm 2 .
次に、本発明のハンダ用メッキ液の製造方法について
詳しく説明する。Next, the method for producing the plating solution for solder of the present invention will be described in detail.
まず、99.99%(4ナイン)以上の品位を有する鉛を
高純度の濃硝酸にて溶解し、該鉛中に含まれるU,Thの放
射性同位元素を錯陰イオンとした後、純水にて遊離硝酸
濃度を5〜10モル濃度に調整して次工程の陰イオン交換
樹脂浄液処理におけるU,Thの吸着効率を向上させ、次い
で該陰イオン交換樹脂浄液処理を行い得られたU,Th含有
量の低減した溶液に上記一般式で表わされる芳香族スル
フオン酸を加え、アルカリにて中和後、濃縮・過・分
離することにより、α線発生量の少ない芳香族スルフオ
ン酸鉛が得られる。同様に、99.99%(4ナイン)以上
の品位を有する錫を高純度の冷希硝酸にて溶解した後遊
離硝酸濃度を5〜10モル濃度に調整して次工程の陰イオ
ン交換樹脂浄液処理におけるU,Thの吸着効率を向上さ
せ、次いで該陰イオン交換樹脂浄液処理を行い得られた
U,Th含有量の低減した溶液に上記一般式で表わされる芳
香族スルフオン酸を加え、アルカリにて中和後、濃縮・
過・分離することにより、α線発生量の少ない芳香族
スルフオン酸錫が得られる。First, lead having a grade of 99.99% (4 nines) or more is dissolved in high-purity concentrated nitric acid, and the radioisotopes of U and Th contained in the lead are converted into complex anions, followed by pure water. The free nitric acid concentration was adjusted to 5 to 10 molar concentration to improve the adsorption efficiency of U and Th in the next step of the anion exchange resin purification treatment, and then the U, Th obtained by performing the anion exchange resin purification treatment was used. The aromatic sulfonate represented by the above general formula is added to the solution having a reduced Th content, neutralized with an alkali, and then concentrated, filtered and separated to obtain a lead aromatic sulfonate having a small amount of α-rays. Can be Similarly, tin having a grade of 99.99% (4 nines) or more is dissolved in high-purity cold dilute nitric acid, and then the concentration of free nitric acid is adjusted to 5 to 10 molar concentration, followed by the next step of anion exchange resin solution treatment. U, Th adsorption efficiency was improved, and then the anion exchange resin purification treatment was performed.
The aromatic sulfonic acid represented by the above general formula is added to the solution having a reduced U and Th content, neutralized with an alkali, and then concentrated and concentrated.
By separating and separating, an aromatic tin sulfonate having a small amount of α-rays can be obtained.
このようにして得られた芳香族スルフオン酸鉛、芳香
族スルフオン酸錫はいずれもU,Thの放射性同位元素の含
有量が20ppb未満であり、かつ放射性α粒子のカウント
数が0.1CPH/cm2未満である。The thus obtained lead aromatic sulfonate and tin aromatic sulfonate have a U, Th radioisotope content of less than 20 ppb, and a radioactive α particle count of 0.1 CPH / cm 2 Is less than.
上記のα線発生量の低い芳香族スルフオン酸鉛、芳香
族スルフオン酸錫及び芳香族スルフオン酸を組成成分と
して含有する水溶液を電解液とし、低α線の放射性ハン
ダ板を陽極に、メツキを行う基板を陰極にそれぞれ接続
することにより、該基板上にα線発生量が少なく、メモ
リーエラー発生を著しく抑制するハンダ合金をメツキす
ることができる。An aqueous solution containing the above-mentioned low α-ray generation amount of aromatic lead sulfonate, tin aromatic sulfonate and aromatic sulfonate as a composition component is used as an electrolytic solution, and plating is performed using a low α-ray radioactive solder plate as an anode. By connecting the substrates to the respective cathodes, it is possible to form a solder alloy on the substrate that generates a small amount of α-rays and significantly suppresses the occurrence of memory errors.
添付図面は本発明の一実施例の断面概略図である。図
において、1はハンダ板,2はメツキ液,3は配線基板であ
る。The attached drawings are schematic sectional views of one embodiment of the present invention. In the figure, 1 is a solder plate, 2 is a plating liquid, and 3 is a wiring board.
次に本発明を実施例によつてより具体的に説明する
が、以下の実施例は本発明の範囲を限定するものではな
い。Next, the present invention will be described more specifically with reference to examples, but the following examples do not limit the scope of the present invention.
実施例1 4ナイン以上の品位を有する鉛濃硝酸で溶解し、純水
で遊離硝酸濃度を、5モル〜10モル濃度に調整し、次い
で該溶液を陰イオン交換樹脂たとえば、ダイヤイオン
(商品名)を充填した塔を通過させ、該溶液中のU,Thを
吸着除去せしめた後、芳香族スルフォン酸としてP−フ
ェノールスルフォン酸を添加し、さらに苛性ソーダ,ま
たはアンモニヤ水で中和後、該溶液を濃縮し、析出した
沈殿を過・分離・乾燥することにより、芳香族スルホ
ン酸鉛を得た。同様に、4ナイン以上の品位を有する錫
を冷希硝酸に溶解し、さらに遊離硝酸濃度を、5モル〜
10モル濃度に調整し、次いで該溶液を陰イオン交換樹脂
にたとえば、ダイヤイオン(商品名)を充填した塔を通
過させ、該溶液中のU,Thを吸着除去せしめた後、芳香族
スルフォン酸としてP−フェノールスルフォン酸を添加
し、さらに苛性ソーダ,またはアンモニヤ水で中和後、
該溶液を濃縮し、析出した沈殿を過・分離・乾燥する
ことにより、芳香族スルフオン酸錫を得た。これら金属
塩の放射性同位元素の含有量を分析したところ、いずれ
も20ppb未満であり、またα粒子のカウント数も0.1CPH/
cm2未満であることが確認された。これら、鉛及び錫の
芳香族スルフオン酸塩をそれぞれ芳香族スルフォン酸
(P−フェノールスルフォン酸)の水溶液に溶解して、
芳香族スルフォン酸、その錫塩および鉛塩を第1表に示
す濃度で含有するハンダ用メッキ液を調製した。得られ
たメッキ液の放射性同元素の含有量および放射性α粒子
のカウント数は、それぞれ第1表に示す通りであった。
このハンダ用メッキ液を用いて、放射性同位元素含有量
20ppb未満でα粒子カウント数0.1CPH/cm2未満であるPb9
0%,Sn10%の組成のハンダ板を陽極に、基板を陰極に、
それぞれ接続し、電流密度60A/cm2としてメッキを行っ
て、基板上に89%Pb−11%Snの組成のハンダ膜を作製し
た。このハンダ膜中のU、Th等の放射性同位元素の含有
量は20ppb未満であり、かつ放射性α粒子のカウント数
が0.1CPH/cm2未満であることが確認された。このメッキ
液を用いて作成したメモリーはソフトエラーの発生が著
しく低下していることが確認された。Example 1 Dissolved in lead-concentrated nitric acid having a grade of 4 nines or more, adjusted the concentration of free nitric acid to 5 to 10 mol with pure water, and then converted the solution to an anion exchange resin such as Diaion (trade name). ) Is passed through a column packed with U) and Th is adsorbed and removed from the solution, P-phenolsulfonic acid is added as aromatic sulfonic acid, and the solution is neutralized with caustic soda or ammonia water. Was concentrated, and the precipitated precipitate was separated, separated and dried to obtain lead aromatic sulfonate. Similarly, tin having a grade of 4 nines or more is dissolved in cold diluted nitric acid, and the concentration of free nitric acid is adjusted to 5 mol or less.
The solution is adjusted to 10 molar concentration, and then the solution is passed through a column filled with, for example, Diaion (trade name) through an anion exchange resin to remove U and Th in the solution by adsorption. After addition of P-phenolsulfonic acid and neutralization with caustic soda or ammonia water,
The solution was concentrated, and the deposited precipitate was separated, separated and dried to obtain an aromatic tin sulfonate. Analysis of the content of radioisotopes in these metal salts showed that all were less than 20 ppb, and the number of α particles was 0.1 CPH /
It was confirmed to be less than cm 2 . These lead and tin aromatic sulfonates are dissolved in an aqueous solution of aromatic sulfonic acid (P-phenolsulfonic acid), respectively.
A plating solution for solder containing aromatic sulfonic acid, its tin salt and lead salt at the concentrations shown in Table 1 was prepared. The content of the radioactive isotope and the count of radioactive α particles in the obtained plating solution were as shown in Table 1, respectively.
Using this solder plating solution, radioisotope content
Is α less than the particle count 0.1CPH / cm 2 at less than 20 ppb PB9
A solder plate with a composition of 0% and Sn 10% is used as an anode, and a substrate is used as a cathode.
Each was connected and plated at a current density of 60 A / cm 2 to form a solder film having a composition of 89% Pb-11% Sn on the substrate. It was confirmed that the content of radioisotopes such as U and Th in the solder film was less than 20 ppb, and the count of radioactive α particles was less than 0.1 CPH / cm 2 . It was confirmed that the memory prepared using this plating solution had significantly reduced occurrence of soft errors.
実施例2 実施例1と同様にして得た、いずれも放射性同位元素
の含有量が20ppb未満、放射性α粒子カウント数が0.1CP
H/cm2未満である芳香族スルフォン酸鉛および芳香族ス
ルフォン酸錫を芳香族スルフォン酸(P−フェノールス
ルフォン酸)の水溶液に溶解して、芳香族スルフォン
酸、その鉛塩および鉛塩を第1表に示す濃度で含有する
ハンダ用メッキ液を調製した。このメッキ液を用いて、
実施例1と同様に低α線の90%Pb−10%Snのハンダ板を
陽極に、基板を陰極にして電解を行い、基板上に89%Pb
−11%Snのハンダ膜を作製した。このハンダ膜中のU、
Th等の放射性同位元素の含有量は20ppb未満であり、か
つ放射性α粒子のカウント数が0.1CPH/cm2未満であるこ
とが確認された。Example 2 A radioisotope content of less than 20 ppb and a radioactive α particle count of 0.1 CP were obtained in the same manner as in Example 1.
An aromatic sulfonic acid, a lead salt thereof, and a lead salt thereof are dissolved in an aqueous solution of aromatic sulfonic acid (P-phenolsulfonic acid) by dissolving lead aromatic sulfonate and tin aromatic sulfonate having an H / cm 2 of less than H / cm 2 . A plating solution for solder containing the concentrations shown in Table 1 was prepared. Using this plating solution,
Electrolysis is performed using a 90% Pb-10% Sn solder plate of low α ray as an anode and a substrate as a cathode in the same manner as in Example 1, and 89% Pb on the substrate.
A solder film of -11% Sn was produced. U in this solder film,
It was confirmed that the content of radioisotopes such as Th was less than 20 ppb, and the count number of radioactive α particles was less than 0.1 CPH / cm 2 .
なお、芳香族スルフオン酸として、P−フエノールス
ルフオン酸、ベンゼンスルフオン酸、P−トルエンスル
フオン酸を使用する実施例、及び同じくP−フエノール
スルフオン酸、ベンゼンスルフオン酸、P−トルエンス
ルフオン酸を使用する比較例を、第1表にそれぞれ実施
例1〜5及び比較例1〜4として併せ示す。実施例1〜
5においては、4ナイン以上の高純度の鉛、錫を硝酸に
溶解させた後、本発明の方法に従って予備精製してから
芳香族スルフォン酸と反応させたのに対し、比較例1〜
4では4ナイン以上の高純度の鉛、錫を硝酸に溶解させ
た後、何ら予備精製せずに芳香族スルフォン酸と反応さ
せたものである。Examples in which P-phenolsulfonate, benzenesulfonate, and P-toluenesulfonate were used as the aromatic sulfonate, and P-phenolsulfonate, benzenesulfonate, and P-toluenesulfonate were also used. Comparative examples using fluoric acid are shown in Table 1 as Examples 1 to 5 and Comparative Examples 1 to 4, respectively. Example 1
In No. 5, lead and tin of high purity of 4 nines or more were dissolved in nitric acid, preliminarily purified according to the method of the present invention, and then reacted with aromatic sulfonic acid.
In No. 4, lead and tin having a high purity of 4 nines or more were dissolved in nitric acid and reacted with aromatic sulfonic acid without any preliminary purification.
比較例5 純水で遊離硝酸濃度を1〜4モルに調整した以外は、
実施例1と同様に、4ナイン以上の品位を有する鉛およ
び錫を使用して、鉛および錫のP−フェノールスルフォ
ン酸塩を調製した。これらの鉛および錫のP−フェノー
ルスルフォン酸塩の放射性同位体元素の含有量はいずれ
も100〜150ppbであり、またα粒子のカウント数は1.3〜
4.9CPH/cm2であることが確認された。 Comparative Example 5 Except that the concentration of free nitric acid was adjusted to 1 to 4 mol with pure water,
As in Example 1, lead and tin P-phenolsulfonates were prepared using lead and tin having a grade of 4 nines or more. The content of radioactive isotopes of these lead and tin P-phenol sulfonates is 100 to 150 ppb, and the count number of α particles is 1.3 to 150 ppb.
It was confirmed to be 4.9 CPH / cm 2 .
実施例1と同様にしてメッキ液を調製し、同様の方法
でメッキを行った。このメッキ板を用いて作成したメモ
リーではソフトエラーの発生が認められた。A plating solution was prepared in the same manner as in Example 1, and plating was performed in the same manner. The occurrence of a soft error was recognized in the memory prepared using this plated plate.
比較例6 純水で遊離硝酸濃度を11〜12モルに調整した以外は、
実施例1と同様に、4ナイン以上の品位を有する鉛およ
び錫を使用して、鉛および錫のP−フェノールスルフォ
ン酸塩を調製した。これらの鉛および錫のP−フェノー
ルスルフォン酸塩の放射性同位体元素の含有量はいずれ
も150〜210ppbであり、またα粒子のカウント数は1.7〜
5.0CPH/cm2であることが確認された。Comparative Example 6 Except that the concentration of free nitric acid was adjusted to 11 to 12 mol with pure water,
As in Example 1, lead and tin P-phenolsulfonates were prepared using lead and tin having a grade of 4 nines or more. The content of the radioactive isotope of these lead and tin P-phenol sulfonates is 150 to 210 ppb, and the count number of α particles is 1.7 to 210 ppb.
It was confirmed to be 5.0 CPH / cm 2 .
実施例1と同様にしてメッキ液を調製し、同様の方法
でメッキを行った。このメッキ板を用いて作成したメモ
リーではソフトエラーの発生が認められた。A plating solution was prepared in the same manner as in Example 1, and plating was performed in the same manner. The occurrence of a soft error was recognized in the memory prepared using this plated plate.
(発明の効果) 本発明は以上から明らかであるように、次の構成要
件、すなわち、 (a) 4ナイン以上の品位を有する鉛及び錫を用いて
純度の高い硝酸で溶解する。(Effects of the Invention) As is clear from the above, the present invention dissolves in high purity nitric acid using lead and tin having a grade of 4 nines or more as follows.
(b) 純水で遊離硝酸濃度を5〜10モル濃度に調整す
る。(B) Adjust the concentration of free nitric acid to 5 to 10 molar with pure water.
(c) 陰イオン交換樹脂浄液処理を行う。(C) Perform anion exchange resin cleaning treatment.
(d) 発生α線量の低い芳香族スルフオン酸鉛,芳香
族スルフオン酸錫塩及び芳香族スルフオン酸を含む水溶
液を電解液とする。(D) An aqueous solution containing lead aromatic sulfonate, tin tin aromatic sulfonate, and aromatic sulfonic acid with low generated α dose is used as the electrolytic solution.
の組合わせからなる、放射性同位元素の含有量が20ppb
未満、かつ放射性α粒子のカウント数が0.1CPH/cm2未満
であることを特徴とする高純度のハンダ用メッキ液の製
造方法を提供するものである。本発明の方法により製造
されたハンダ用メッキ液を使用することによつてメモリ
ーエラーの発生を著しく抑制するハンダ膜を形成するこ
とができるので、大容量メモリー素子である256K RAM
式或はそれ以上のメモリーや各種超LSI等の半導体装置
の部品、基板等にハンダ用合金をメツキすることが可能
である。20 ppb radioisotope content
The present invention provides a method for producing a high-purity plating solution for solder, wherein the count is less than 0.1 CPH / cm 2 . By using a solder plating solution manufactured by the method of the present invention, a solder film can be formed which significantly suppresses the occurrence of memory errors.
It is possible to apply a solder alloy to parts of a semiconductor device such as a memory of a formula or more or various super LSIs, a substrate, and the like.
図面は本発明のメツキ液を収納した電解槽の断面図であ
る。図において、1はハンダ板,2はメツキ液,3は配線基
板である。The drawing is a sectional view of an electrolytic cell containing the plating solution of the present invention. In the figure, 1 is a solder plate, 2 is a plating liquid, and 3 is a wiring board.
フロントページの続き (56)参考文献 特開 昭59−227722(JP,A) 特開 昭62−6793(JP,A) 特公 昭49−16176(JP,B1)Continuation of the front page (56) References JP-A-59-227722 (JP, A) JP-A-62-6793 (JP, A) JP-B-49-16176 (JP, B1)
Claims (1)
ぞれ水素原子、水酸基、低級アルキル基及びスルフォン
酸基よりなる群の中から選ばれる)で表わされる芳香族
スルフォン酸ならびに該芳香族スルフォン酸の鉛塩およ
び錫塩を含有するハンダ用メッキ液の製造方法であっ
て、下記〜の工程からなることを特徴とする、放射
性同位元素の含有量が20ppb未満で、放射性α粒子のカ
ウント数が0.1CPH/cm2未満のハンダ用メッキ液の製造方
法。 純度が99.99%以上の鉛および/または錫を高純度硝
酸水溶液に溶解し、 得られた溶液の遊離硝酸濃度を5〜10モルに調整し、 濃度調整した溶液を陰イオン交換樹脂で精製して、溶
液中のUおよびThの含有量を低減させ、 精製した溶液に芳香族スルフォン酸を反応させた後、
中和および濃縮し、析出した沈殿を分離および乾燥し
て、芳香族スルフォン酸鉛および芳香族スルフォン酸錫
を取得し、 こうして得た芳香族スルフォン酸鉛と芳香族スルフォ
ン酸錫を、前記芳香族スルフォン酸を含む水溶液に溶解
させる。1. The following general formula: Wherein R 1 and R 2 may be the same or different and each is selected from the group consisting of a hydrogen atom, a hydroxyl group, a lower alkyl group and a sulfonic acid group, and the aromatic sulfonic acid represented by the formula A method for producing a solder plating solution containing a lead salt and a tin salt of an aromatic sulfonic acid, characterized by comprising the following steps, wherein the content of the radioisotope is less than 20 ppb, A method for producing a plating solution for solder having a count of less than 0.1 CPH / cm 2 . Dissolve lead and / or tin with a purity of 99.99% or more in a high-purity nitric acid aqueous solution, adjust the free nitric acid concentration of the obtained solution to 5 to 10 mol, and purify the concentration-adjusted solution with an anion exchange resin. Reducing the content of U and Th in the solution, and reacting the purified solution with aromatic sulfonic acid,
It is neutralized and concentrated, and the deposited precipitate is separated and dried to obtain lead aromatic sulfonate and tin aromatic sulfonate. The thus obtained lead aromatic sulfonate and tin aromatic sulfonate are separated from the aromatic sulfonate. Dissolve in an aqueous solution containing sulfonic acid.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62083673A JP2590869B2 (en) | 1987-04-04 | 1987-04-04 | Manufacturing method of plating solution for solder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62083673A JP2590869B2 (en) | 1987-04-04 | 1987-04-04 | Manufacturing method of plating solution for solder |
Publications (2)
Publication Number | Publication Date |
---|---|
JPS63250485A JPS63250485A (en) | 1988-10-18 |
JP2590869B2 true JP2590869B2 (en) | 1997-03-12 |
Family
ID=13808999
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62083673A Expired - Lifetime JP2590869B2 (en) | 1987-04-04 | 1987-04-04 | Manufacturing method of plating solution for solder |
Country Status (1)
Country | Link |
---|---|
JP (1) | JP2590869B2 (en) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9666547B2 (en) | 2002-10-08 | 2017-05-30 | Honeywell International Inc. | Method of refining solder materials |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP4582294B2 (en) * | 2004-04-02 | 2010-11-17 | 三菱マテリアル株式会社 | Lead-tin alloy solder plating solution |
JP6009218B2 (en) * | 2011-05-24 | 2016-10-19 | ローム アンド ハース エレクトロニック マテリアルズ エルエルシーRohm and Haas Electronic Materials LLC | Alpha particle emitter removal |
Family Cites Families (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS4916176A (en) * | 1972-06-07 | 1974-02-13 | ||
JPS59227722A (en) * | 1983-05-09 | 1984-12-21 | Mitsubishi Metal Corp | Lead oxide for low-melting glass for sealing semiconductor device and its preparation |
JPS626793A (en) * | 1985-07-03 | 1987-01-13 | Mitsubishi Metal Corp | Pb alloy powder for solder paste |
-
1987
- 1987-04-04 JP JP62083673A patent/JP2590869B2/en not_active Expired - Lifetime
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US9666547B2 (en) | 2002-10-08 | 2017-05-30 | Honeywell International Inc. | Method of refining solder materials |
Also Published As
Publication number | Publication date |
---|---|
JPS63250485A (en) | 1988-10-18 |
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