JP2754030B2 - Manufacturing method of high purity tin - Google Patents
Manufacturing method of high purity tinInfo
- Publication number
- JP2754030B2 JP2754030B2 JP4855789A JP4855789A JP2754030B2 JP 2754030 B2 JP2754030 B2 JP 2754030B2 JP 4855789 A JP4855789 A JP 4855789A JP 4855789 A JP4855789 A JP 4855789A JP 2754030 B2 JP2754030 B2 JP 2754030B2
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- JP
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- Prior art keywords
- tin
- sulfuric acid
- hydrochloric acid
- electrolysis
- electrolytic solution
- Prior art date
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Description
【発明の詳細な説明】 ［産業上の利用分野］ 本発明は、主としてエレクトロニクス産業分野におい
て用いられるロー付け材や半田材料等として有用な高純
度、かつα線カウントの少ない錫の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing tin having high purity and low α-ray count, which is useful mainly as a brazing material or a solder material used in the electronics industry.
［従来の技術および発明が解決しようとする課題］ 近来、エレクトロニクス分野における技術の進歩は著
しく、ICはより大容量化へと向い、半導体メモリにおい
ても1Mビットから4MビットDRAMへと開発は進んできた。
それらを高性能、高信頼度とするためにIC組立等に用い
られるロー付け材や半田材料として用いられる錫にも高
純度化、低α線化が要求されるのは必至である。[Problems to be Solved by Conventional Techniques and Inventions] In recent years, the technological progress in the electronics field has been remarkable, and ICs have been moving toward larger capacities, and the development of semiconductor memories from 1 Mbit to 4 Mbit DRAMs has been progressing. Was.
In order to obtain high performance and high reliability, it is inevitable that the brazing material used for IC assembly and the like and the tin used as a solder material also need to have high purity and low α ray.
高純度の錫を得るには、電解を繰返すか、あるいは仕
上げに真空蒸留やゾーン精製といった乾式精製が行なわ
れている。しかし、前者の方法では錫中に含まれるPb,I
n等の不純物は数ppmオーダーにとどまり、錫の高純度化
は達成し得ず、また電解を繰返すために、煩雑で生産性
に劣り、コスト的にも不利である。また後者の方法は電
力経費が嵩み、実操業を考えた場合に問題がある。In order to obtain high-purity tin, electrolysis is repeated, or dry purification such as vacuum distillation or zone purification is performed for finishing. However, in the former method, Pb, I contained in tin
Impurities such as n are only on the order of a few ppm, so that high purity of tin cannot be achieved, and since the electrolysis is repeated, it is complicated, poor in productivity and disadvantageous in cost. In addition, the latter method has a problem in that electric power costs are increased and actual operation is considered.
この課題を解決すべくため、本発明者等によって特願
昭63−110436号において、精製度の高い硫酸を一定量含
有する電解液を用いる方法が提案されている。しかし、
この方法においてもα線カウントの低減は充分でなく、
またPb等の不純物が残存し、高純度化といった観点から
も課題があった。In order to solve this problem, the present inventors have proposed in Japanese Patent Application No. 63-110436 a method using an electrolytic solution containing a fixed amount of sulfuric acid having a high degree of purification. But,
Even in this method, the reduction of the α-ray count is not enough,
In addition, impurities such as Pb remain, and there is a problem from the viewpoint of high purity.
本発明は、上記課題に鑑み、高純度でα線カウントが
極めて少なく、しかも簡便かつ安価な錫の製造方法を提
供することを目的とするものである。In view of the above problems, an object of the present invention is to provide a simple and inexpensive method for producing tin, which has a high purity, an extremely small α-ray count, and is inexpensive.
［課題を解決するための手段及び作用］ 本発明者等は、上記目的を達成するために種々検討を
重ねた結果、精製度の高い硫酸と塩酸が一定割合で含有
された電解液を用い、かつ高純度の錫を陽極として配置
して電解を行なうことにより、上記目的を達成し得るこ
とを知見して本発明に到達した。[Means and Actions for Solving the Problems] The present inventors have conducted various studies in order to achieve the above object, and as a result, using an electrolytic solution containing sulfuric acid and hydrochloric acid with a high degree of purification at a fixed ratio, The inventors have found that the above object can be achieved by arranging high-purity tin as an anode and performing electrolysis, and arrived at the present invention.
すなわち、本発明の錫の製造方法は、JIS Ｋ 8951
に規定される試薬一級硫酸の規格に少なくとも適合する
硫酸90〜240g/とJIS Ｋ 8180に規定される試薬一級
塩酸の規格に少なくとも適合する塩酸10〜50g/を含有
する電解液中で、純度が99.97重量％以上である錫を陽
極に用いて電解を行なうことを特徴とする。That is, the method for producing tin of the present invention is based on JIS K 8951
In an electrolyte containing 90 to 240 g / sulfuric acid that meets at least the standard of reagent primary sulfuric acid specified in JIS K10 and 10 to 50 g / hydrochloric acid that meets at least the standard of reagent primary hydrochloric acid specified in JIS K8180, the purity is Electrolysis is performed using tin of 99.97% by weight or more as an anode.
本発明では、電解液中に硫酸と塩酸が含有される。こ
こで用いられる硫酸はJIS Ｋ 8951に規定される試薬
一級硫酸の規格に少なくとも適合する硫酸で、同規格の
硫酸あるいはそれ以上に精製された硫酸である。また、
ここに用いられる塩酸はJIS Ｋ 8180に規定される試
薬一級塩酸の規格に少なくとも適合する塩酸で、同規格
の塩酸あるいはそれ以上に精製された塩酸である。これ
らの硫酸、塩酸は上記JIS規格を少なくとも満たすもの
であれば、市販品でも自家精製品のいずれであってもよ
い。In the present invention, the electrolytic solution contains sulfuric acid and hydrochloric acid. The sulfuric acid used here is a sulfuric acid which conforms at least to the reagent primary sulfuric acid standard specified in JIS K 8951, and is a sulfuric acid purified to the same standard or higher. Also,
The hydrochloric acid used here is a hydrochloric acid that conforms at least to the standard for reagent primary hydrochloric acid specified in JIS K 8180, and is hydrochloric acid of the same standard or purified to a higher level. These sulfuric acid and hydrochloric acid may be either commercial products or self-purified products as long as they satisfy at least the above JIS standards.
本発明において、電解液中の硫酸、塩酸のいずれかが
上記規格を満たさない場合には、本願発明で目的とする
錫の高純度化やα線カウントの低減化は達成されない。In the present invention, when either sulfuric acid or hydrochloric acid in the electrolytic solution does not satisfy the above-mentioned standard, the purifying of tin and the reduction of α-ray count, which are the objects of the present invention, cannot be achieved.
本発明における電解液中の硫酸濃度および塩酸濃度は
不純物をより低減させるために重要であり、特に塩酸濃
度は錫中の不純物である鉛含有量に影響を与え、一般に
は塩酸濃度が高い程、錫中の鉛含有量が低下する。ま
た、塩酸濃度は電解液の電解電圧を左右する要素でもあ
る。The sulfuric acid concentration and the hydrochloric acid concentration in the electrolytic solution in the present invention are important for further reducing impurities, and in particular, the hydrochloric acid concentration affects the lead content, which is an impurity in tin. The lead content in tin decreases. Further, the hydrochloric acid concentration is also a factor that determines the electrolysis voltage of the electrolytic solution.
本発明において、電解液中の硫酸濃度は90〜240g/
、好ましくは120〜240g/である。硫酸濃度が90g/
未満の場合は、陰極への析出錫のα線カウントが高く、
析出錫中のSb含有量が高くなり、240g/を超える場合
は、陽極である錫の電解液中への溶出が激しくなり、析
出錫の純度が劣化するので好ましくない。In the present invention, the sulfuric acid concentration in the electrolytic solution is 90 to 240 g /
, Preferably 120 to 240 g /. Sulfuric acid concentration is 90g /
If less than, the α-ray count of the deposited tin on the cathode is high,
If the Sb content in the deposited tin increases and exceeds 240 g /, the elution of tin as an anode into the electrolytic solution becomes severe and the purity of the deposited tin deteriorates, which is not preferable.
また、電解液中の塩酸濃度は10〜50g/、好ましくは
20〜30g/である。塩酸濃度が10g/未満では、液中の
鉛許容量が少ないため析出錫中に鉛含有量が高くなり、
50g/を超えると塩素ガスが発生するため好ましくな
い。The hydrochloric acid concentration in the electrolyte is 10 to 50 g /, preferably
20-30 g /. If the concentration of hydrochloric acid is less than 10 g /, the lead content in the deposited tin becomes high because the lead tolerance in the liquid is small,
If it exceeds 50 g /, chlorine gas is generated, which is not preferable.
この硫酸、塩酸を希釈して電解液を作成する際に用い
られる水は、放射線物質を含有しない高純度水が好まし
い。The water used for preparing the electrolytic solution by diluting the sulfuric acid and hydrochloric acid is preferably high-purity water containing no radioactive substance.
また、本発明に用いられる電解液中の錫イオン濃度は
15〜50g/であることが望ましい。15g/未満の場合は
陰極への析出錫が稠密でなくなり、50g/を超える場合
は経済性が悪くなる。Further, the tin ion concentration in the electrolytic solution used in the present invention is
It is desirably 15 to 50 g /. If it is less than 15 g /, the tin deposited on the cathode will not be dense, and if it exceeds 50 g /, the economic efficiency will be poor.
さらに、この電解液にゼラチンを0.5〜1.0g/を添加
すると、陰極に析出する錫の析出状態の改善に効果があ
る。Further, when 0.5 to 1.0 g / gelatin is added to this electrolytic solution, it is effective in improving the state of deposition of tin deposited on the cathode.
このような成分を含有する本発明で用いられる電解液
は、電解中は電解槽内での濃度不均一を防止するために
循環を行なうことが望ましい。It is desirable that the electrolytic solution containing such components used in the present invention be circulated during electrolysis in order to prevent concentration unevenness in the electrolytic cell.
本発明で陽極として用いられる錫は、純度が99.97重
量％以上であることが必要である。純度が99.97重量％
未満の錫の場合はα線カウントが高くなる。Tin used as the anode in the present invention must have a purity of 99.97% by weight or more. Purity 99.97% by weight
In the case of less than tin, the α-ray count increases.
本発明にあっては、上述の電解液および陽極を用いて
電解を行なうが、その際に高純度の錫からなる陽極を耐
酸性の化学繊維を両面に貼付した隔離箱に装入して、陽
極泥を回収する。また、陰極としては、ステンレス等の
金属板が用いられるが、本発明の製造方法により一度陰
極に析出させた錫を加工して用いることも可能である。In the present invention, the electrolysis is performed using the above-described electrolyte solution and the anode.At that time, the anode made of high-purity tin is charged into an isolation box having acid-resistant chemical fibers attached to both sides, Collect the anode mud. Further, a metal plate such as stainless steel is used as the cathode, but it is also possible to process and use tin once deposited on the cathode by the production method of the present invention.
この際の電解条件は、電解液の温度は15〜95℃、電流
密度は0.3〜1.0A/dm2であることが好ましい。電解液の
温度が15℃未満では電解液の電気的抵抗が高いため電解
効率が悪くなり、また添加剤の効果が半減する。また95
℃を超えると電解液が沸騰した状態となってしまうた
め、それぞれ好ましくない。さらに、電解液を特に加温
しなくても15℃以上であれば電解が良好に続くので経済
的な面で電解液の温度はより低い方が好適である。The electrolysis conditions at this time are preferably such that the temperature of the electrolytic solution is 15 to 95 ° C. and the current density is 0.3 to 1.0 A / dm 2 . If the temperature of the electrolytic solution is lower than 15 ° C., the electric resistance of the electrolytic solution is high, so that the electrolytic efficiency is deteriorated and the effect of the additive is reduced by half. Also 95
If the temperature exceeds ℃, the electrolyte will be in a boiling state, which is not preferable. Further, if the temperature is 15 ° C. or more without particularly heating the electrolytic solution, the electrolysis continues favorably. Therefore, it is preferable that the temperature of the electrolytic solution is lower in terms of economy.
電解時の電流密度が0.3A/dm2未満の場合は陰極に析出
させる錫に悪い影響はないものの、単位時間当りの取得
量が少なく非能率的であり、1.0A/dm2を超える場合は陽
極の不働態化を早く招くのでそれぞれ好ましくない。Although current density during electrolysis in the case of less than 0.3 A / dm 2 is not bad influence on the tin to be deposited on the cathode, obtaining the amount per unit time is less inefficient, if it exceeds 1.0A / dm 2 is It is not preferable because passivation of the anode is quickly caused.
この様な本発明の製造方法によると純度99.998重量％
以上、α線カウント数が0.005C/hr・cm2以下、不純物で
あるPb含有量が1ppm未満で、しかもその他の不純物であ
るIn,Cu,Bi,As,Sb,Feのいずれの含有量も1ppm未満の錫
が得られる。According to the production method of the present invention, the purity is 99.998% by weight.
Above, the α-ray count is 0.005 C / hrcm 2 or less, the content of Pb as an impurity is less than 1 ppm, and the content of any of the other impurities In, Cu, Bi, As, Sb, Fe Less than 1 ppm of tin is obtained.
［作用］ 先に出願した特願昭63−110436号に記載されている一
定量の硫酸を用いた電解液より、一定量の硫酸と塩酸を
用いた電解液のほうがα線放射の主原因となるウラン、
トリウム等の放射性物質やラジウム、ラドン、ポロニウ
ム、ビスマス、アスタチン、鉛等の崩壊系列に属する放
射性の状態にある放射性物質の系外への除去が一層なさ
れるため、α線カウントが0.005C/hr・cm2以下になり、
また硫酸と塩酸との混合液であるため液中の鉛許容量が
高くなり、従って、析出錫中の不純物であるPbの含有量
も1ppm未満となったものと考えられる。[Effect] An electrolyte using a certain amount of sulfuric acid and hydrochloric acid is a main cause of α-ray emission than an electrolyte using a certain amount of sulfuric acid described in Japanese Patent Application No. 63-110436 previously filed. Uranium,
Radioactive substances such as thorium and radium, radon, polonium, bismuth, astatine, lead and other radioactive substances belonging to the decay series are further removed from the system, so that the α-ray count is 0.005 C / hr.・ Below cm 2
Further, it is considered that the allowable amount of lead in the liquid was high because of the mixed liquid of sulfuric acid and hydrochloric acid, and therefore, the content of Pb, which is an impurity in the deposited tin, was also less than 1 ppm.
［実施例］ 以下本発明を実施例および比較例に基づき、具体的に
説明する。[Examples] Hereinafter, the present invention will be specifically described based on Examples and Comparative Examples.
実施例１〜６ 第１表に示される規格の硫酸と塩酸並びに錫を含有
し、硫酸と塩酸の濃度が第１表に示す濃度で、錫濃度が
20g/の電解液を用い、約55ml/minの速度で約５の電
解層中を循環させ電解を行なった。この電解に際し、純
度99.97重量％錫を10×10×1.5cmに鋳込んで陽極とし、
10×10×0.2cmのステンレス板を陰極とした。電解条件
は電流密度を0.4A/dm2、室温で電解行なった。Examples 1 to 6 contain sulfuric acid, hydrochloric acid and tin of the specifications shown in Table 1, the concentrations of sulfuric acid and hydrochloric acid are those shown in Table 1, and the tin concentration is
Electrolysis was carried out by circulating through about 5 electrolytic layers at a rate of about 55 ml / min using an electrolytic solution of 20 g / min. At the time of this electrolysis, 99.97% by weight of tin was cast into 10 × 10 × 1.5cm tin to form an anode,
A 10 × 10 × 0.2 cm stainless plate was used as the cathode. Electrolysis was carried out at a current density of 0.4 A / dm 2 and at room temperature.
上記した電解液は、実施例１にあって硫酸錫溶液に塩
酸を添加して調製し、実施例２〜６では塩化錫溶液に硫
酸添加した。また、上記電解液にはゼラチンを通電前に
1g/添加し、通電中は常時0.5g/day滴下した。また、
この陽極は、陽極泥回収のために耐酸性の化学繊維を両
面に貼付した隔離箱内に装入し、陰極は剥離状態を良く
するためにサンドペーパー2000番で仕上げた。The electrolytic solution described above was prepared by adding hydrochloric acid to the tin sulfate solution in Example 1, and in Examples 2 to 6, sulfuric acid was added to the tin chloride solution. Also, gelatin should be added to the above electrolyte before energizing.
1 g / addition was conducted, and 0.5 g / day was constantly dropped during energization. Also,
The anode was placed in an isolation box with acid-resistant chemical fibers stuck on both sides to collect the anode mud, and the cathode was finished with sandpaper No. 2000 to improve the peeling state.
電解後、陰極上に析出した錫を剥離し、水洗、乾燥
後、α線測定器でα線カウントを測定すると同時に、錫
中の鉛含有量の定量分析を行なった。その結果を第１表
に示す。After the electrolysis, the tin deposited on the cathode was peeled off, washed with water and dried, and the α-ray count was measured with an α-ray measuring device, and at the same time, the lead content in tin was quantitatively analyzed. Table 1 shows the results.
比較例１〜２ 実施例１〜６で用いた硫酸と塩酸を含有する電解液に
代えて、第１表に示す濃度の硫酸錫溶液を含有する電解
液を用い、その他の条件は実施例１〜６とすべて同様に
電解を行なった。Comparative Examples 1 and 2 Instead of the electrolyte solution containing sulfuric acid and hydrochloric acid used in Examples 1 to 6, an electrolyte solution containing a tin sulfate solution having a concentration shown in Table 1 was used. Electrolysis was carried out in the same manner as in Nos. 6 to 6.
電解後、陰極上に析出した錫を剥離し、水洗、乾燥
後、α線測定器でα線カウントを測定すると同時に、錫
中の鉛含有量の定量分析を行なった。その結果を第１表
に示す。After the electrolysis, the tin deposited on the cathode was peeled off, washed with water and dried, and the α-ray count was measured with an α-ray measuring device, and at the same time, the lead content in tin was quantitatively analyzed. Table 1 shows the results.
第１表に示されるように、硫酸と塩酸を含有する電解
液で電解を行なった実施例１〜６は、析出した錫のα線
カウントは、0.005C/hr・cm2以下であり、錫中の鉛含有
量も1ppm未満となった。また、電解液の調製方法に拘ら
ず、電解電圧は降下し、錫中のα線カウントや鉛含有量
が少ない錫が得られることが判る。 As shown in Table 1, in Examples 1 to 6 in which electrolysis was performed using an electrolytic solution containing sulfuric acid and hydrochloric acid, the α ray count of the deposited tin was 0.005 C / hr · cm 2 or less, The lead content in it was also less than 1 ppm. In addition, it can be seen that regardless of the method of preparing the electrolytic solution, the electrolytic voltage drops, and tin having a small α-ray count and lead content in tin can be obtained.
これに対して、硫酸のみを含有する電解液で電解を行
なった比較例１〜２は、析出した錫のα線カウントは0.
006〜0.008C/hr・cm2、錫中の鉛含有量は20〜30ppmであ
り、実施例１〜６に比較して錫中のα線カウントや鉛含
有量は高い値を示す。また、電解電圧も実施例１〜６に
比較して高いことが判る。On the other hand, in Comparative Examples 1 and 2 in which electrolysis was performed using an electrolytic solution containing only sulfuric acid, the α-ray count of the deposited tin was 0.3.
006 to 0.008 C / hr · cm 2 , the lead content in tin is 20 to 30 ppm, and the α ray count and the lead content in tin show higher values than those in Examples 1 to 6. Also, it can be seen that the electrolysis voltage is higher than in Examples 1 to 6.
［発明の効果］ 以上説明した様に、精製度の高い硫酸および塩酸が一
定割合で含有された電解液を用い、かつ高純度の錫を陽
極として配置して電解する本発明の製造方法によって、
析出した鉛のα線カウントが0.005C/hr・cm2以下、鉛濃
度が1ppm未満と従来の錫と比較してα線カウントが低
く、しかも高純度のものが効率よく得られる。[Effects of the Invention] As described above, according to the production method of the present invention in which an electrolytic solution containing sulfuric acid and hydrochloric acid having a high degree of purification at a fixed ratio is used, and high-purity tin is arranged as an anode to perform electrolysis.
When the α-ray count of the precipitated lead is 0.005 C / hr · cm 2 or less and the lead concentration is less than 1 ppm, the α-ray count is lower than that of conventional tin, and a highly pure product can be obtained efficiently.
このようにして得られた錫を大容量の半導体メモリー
組立時のロー付け材や半田材料等として用いることによ
り、半導体メモリー等のソフトエラを低減させ、電子機
器の信頼度を向上させることが可能である。By using the tin obtained in this way as a brazing material or a solder material when assembling a large-capacity semiconductor memory, it is possible to reduce soft errors of the semiconductor memory and the like and improve the reliability of electronic devices. is there.
Claims (1)
の規格に少なくとも適合する硫酸90〜240g/とJIS Ｋ
8180に規定される試薬一級塩酸の規格に少なくとも適
合する塩酸10〜50g/を含有する電解液中で、純度が9
9.97重量％以上である錫を陽極に用いて電解を行なうこ
とを特徴とする錫の製造方法。(1) 90-240 g / sulfuric acid, which meets at least the standard of primary sulfuric acid of reagent specified in JIS K 8951, and JIS K
In an electrolyte containing 10 to 50 g / hydrochloric acid, which meets at least the specification of reagent primary hydrochloric acid specified in 8180, purity is 9
A method for producing tin, characterized in that electrolysis is carried out by using 9.97% by weight or more of tin as an anode.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4855789A JP2754030B2 (en) | 1989-03-02 | 1989-03-02 | Manufacturing method of high purity tin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4855789A JP2754030B2 (en) | 1989-03-02 | 1989-03-02 | Manufacturing method of high purity tin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02228487A JPH02228487A (en) | 1990-09-11 |
| JP2754030B2 true JP2754030B2 (en) | 1998-05-20 |
Family
ID=12806684
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4855789A Expired - Lifetime JP2754030B2 (en) | 1989-03-02 | 1989-03-02 | Manufacturing method of high purity tin |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2754030B2 (en) |
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| Publication number | Publication date |
|---|---|
| JPH02228487A (en) | 1990-09-11 |
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