JPH01104793A - Vatting method for nonaqueous electrolytic aluminizing bath - Google Patents

Vatting method for nonaqueous electrolytic aluminizing bath

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Publication number
JPH01104793A
JPH01104793A JP26049387A JP26049387A JPH01104793A JP H01104793 A JPH01104793 A JP H01104793A JP 26049387 A JP26049387 A JP 26049387A JP 26049387 A JP26049387 A JP 26049387A JP H01104793 A JPH01104793 A JP H01104793A
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JP
Japan
Prior art keywords
plating
inert gas
tank
mixing
vessel
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
Application number
JP26049387A
Other languages
Japanese (ja)
Other versions
JP2623482B2 (en
Inventor
Setsuko Takahashi
節子 高橋
Kumiko Mori
森 久美子
Kikuko Akimoto
秋元 菊子
Ryozo Akama
赤間 良三
Isao Saeki
功 佐伯
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nippon Steel Nisshin Co Ltd
Original Assignee
Nisshin Steel Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Nisshin Steel Co Ltd filed Critical Nisshin Steel Co Ltd
Priority to JP62260493A priority Critical patent/JP2623482B2/en
Publication of JPH01104793A publication Critical patent/JPH01104793A/en
Application granted granted Critical
Publication of JP2623482B2 publication Critical patent/JP2623482B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Electroplating And Plating Baths Therefor (AREA)

Abstract

PURPOSE:To safely remove impurities even when a large amt. is vatted by mixing AlCl3 and butylpyridium chloride in an inert gas atmosphere, substituting the impurities for Al, and then filtering a plating soln. CONSTITUTION:The air in a chemical feed vessel 5, a mixing vessel 1, a refining vessel 10, and a storage vessel 15 is replaced by an inert gas. AlCl2 and butylpyridium chloride are charged in the mixing vessel 1 in a specified ratio, mixed by an agitator 6, and melted to prepare the plating soln. The plating soln. is dropped into the refining vessel 10, the impurities in the plating soln. are substituted and deposited on an Al wire 12, and the soln. is refined. The refined plating soln. is filtered by a filter 13, and transferred to the storage vessel 15. When electroplating is carried out by using the refined plating soln., a high-purity Al plating layer can be formed.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明は、塩化アルミニウムとブチルピリジニウムクロ
リドとの溶融塩浴を用いる電気アルミニウムめっき浴の
11!浴方法およびその装置に関する。
Detailed Description of the Invention (Industrial Application Field) The present invention provides 11! of an electrolytic aluminum plating bath using a molten salt bath of aluminum chloride and butylpyridinium chloride. This invention relates to a bathing method and apparatus.

(従来技術) 塩化アルミニウムを使用する非水溶液めっき浴での電気
アルミニウムめっき方法としては、従来、(1)AIC
I、とLi^llI4またはLiHとをエーテルに溶解
しためっき浴を用いる方法、(2ンΔIC1,とLiA
l11゜とをテトラヒドロフランに溶解しためっき浴を
用いる方法、さらには、(3)ハロゲン化アルミニウム
とフルキルピリジニウムハロゲン化物との’II 1m
塩浴を用いる方法などが知られている。
(Prior Art) As an electrolytic aluminum plating method in a non-aqueous plating bath using aluminum chloride, conventionally, (1) AIC
A method using a plating bath in which I and Li^llI4 or LiH are dissolved in ether (2-ΔIC1, and LiA
11° in tetrahydrofuran; and (3) 'II 1m of aluminum halide and furkylpyridinium halide.
A method using a salt bath is known.

これらのめっき浴の建浴は、(1)、(2)の方法の場
合、LiAl11.やLiHが酸素に触れると発火する
ので、溶解を不活性ガス雰皿気下で行い、溶解後ろ過す
る方法で行なわれている。
In the case of methods (1) and (2), these plating baths are prepared using LiAl11. Since LiH and LiH ignite when exposed to oxygen, they are melted in an inert gas atmosphere and filtered after melting.

また、(3)の方法の場合のめっき浴も、イオンが酸素
に触れると、酸化されるので、不活性ガス雰囲気下で行
い、ろ過していた。
Furthermore, the plating bath used in method (3) was also oxidized when the ions came into contact with oxygen, so the plating bath was carried out under an inert gas atmosphere and filtered.

(発明が解決しようとする問題、α) しかし、(3)の一方法の場合、塩化アルミニウムとブ
チルピリジニウムクロリドを一度に密閉容器内で多量に
建浴すると、著しい発熱を伴う場合があり、危険であっ
た。また、塩化アルミニウムは、試薬、工業薬品として
も、通常不純物が含まれているため、めっき液を最後に
ろ過しただけでは、Fe、 Pb、lI20などの不純
物を除去できないものであった。このため、高純度の^
1めっきを行うことができず、純度は、99.00%程
度が限界で、高純度のΔ1めっきを必要とする用途のも
のをめっきできないという問題があった。
(Problem to be solved by the invention, α) However, in the case of method (3), if large amounts of aluminum chloride and butylpyridinium chloride are prepared at once in a closed container, significant heat generation may occur, which is dangerous. Met. Furthermore, aluminum chloride, even as a reagent or an industrial chemical, usually contains impurities, so impurities such as Fe, Pb, and 1I20 cannot be removed just by filtering the plating solution at the end. For this reason, high purity
There was a problem in that it was not possible to perform Δ1 plating, and the purity was limited to about 99.00%, making it impossible to plate for applications that required high purity Δ1 plating.

そこで、本発明では、同時に多量に建浴しても安全で、
不純物を除去できる建浴方法および連続建浴装置を提供
するもの′である。
Therefore, in the present invention, it is safe to prepare a large amount of bath at the same time,
The present invention provides a bath preparation method and a continuous bath preparation device capable of removing impurities.

(問題点を解決するための手段) 本発明は、塩化アルミニウムとブチルピリジニウムクロ
リドとを不活性ガス雰囲気下で所定の比率で混合した後
、同雰囲気下で金属アルミニウムに接触させて置換反応
により不純物を除去し、しかる後にフィルターでろ過す
る方法により建浴するようにした。
(Means for Solving the Problems) The present invention involves mixing aluminum chloride and butylpyridinium chloride in a predetermined ratio under an inert gas atmosphere, and then bringing the mixture into contact with metallic aluminum under the same atmosphere to remove impurities through a substitution reaction. The bath was prepared by removing the water and then filtering it with a filter.

そして、この建浴装置として、攪袢機と冷却器とを備え
、かつ、上部に開閉自在な投入口が設けられた混合槽と
、加熱器を備え、内部に金属アルミ、ニウムが装入され
た精製槽とが配管により接続され、さらに、この精製槽
とめっき液の貯蔵槽がろ過装置を有する配管で接続され
ていて、これらの各相は、密閉型で、上部に不活性ガス
の導入排出口が設けられている建浴装置を発明した。
The bath preparation device is equipped with a stirrer and a cooler, a mixing tank with an input port that can be opened and closed at the top, and a heater, and metal aluminum and aluminum are charged inside. The purification tank is connected by piping, and the purification tank and the plating solution storage tank are connected by piping equipped with a filtration device. Invented a bath preparation device equipped with an outlet.

本発明での建浴は、塩化アルミニウム(^IC1,と記
す)とブチルピリジニウムクロリド(以下Bf’Cと略
記する)とを計量して、これらを従来のように不活性ガ
ス雰囲気下で混合する。この混合により^IC1,と[
lI’Cは、ともに固体であるが、溶融し、常温でも液
体なめっき液となる。この混合の際、発熱するので、密
閉′t、器内で一度に多量に混合する場合は、冷却する
ようにする。
To prepare a bath in the present invention, aluminum chloride (denoted as ^IC1) and butylpyridinium chloride (hereinafter abbreviated as Bf'C) are weighed and mixed under an inert gas atmosphere as in the conventional method. . This mixture produces ^IC1, and [
Although lI'C is both solid, it melts and becomes a liquid plating solution even at room temperature. During this mixing, heat is generated, so if a large amount is mixed at once in a sealed vessel, be sure to cool it.

混合後は、不活性がス雰囲気下で金属Δ1と接触させる
。この接触によりAlCl、中に含まれCいるFe5P
I3、I20などの不純物は金属^1に置換析出し、精
5!!される。この精製の際、めっき液が常温であると
、精製時間が長くなるので、金属^1を両極にして0.
5^/dm2以下の低電流密度で電解したり、めっき液
温度を100℃前後に高くしたりすると、精製時間を短
縮できる。めっき液を金属^1に接触させる方法として
は、めっき液中に金属^1(例えば^1ワイヤー)を投
入してもよく、予め金iAIを装入しである容器の中に
めっき液を入るようにしてもよい。
After mixing, the mixture is brought into contact with the metal Δ1 under an inert gas atmosphere. Due to this contact, AlCl, Fe5P contained in it
Impurities such as I3 and I20 are substituted and precipitated by metal ^1, and the precision 5! ! be done. During this purification, if the plating solution is at room temperature, the purification time will be longer, so the metal ^1 is used as both poles and 0.
Purification time can be shortened by electrolyzing at a low current density of 5^/dm2 or less or by increasing the plating solution temperature to around 100°C. As a method of bringing the plating solution into contact with the metal ^1, the metal ^1 (for example, ^1 wire) may be introduced into the plating solution, and the plating solution is poured into a container that has been charged with gold iAI in advance. You can do it like this.

4を属^iにより精製しためっき液は、ろ過し、不活性
ガス雰囲気の充たされた貯N!L槽に保管しておけばよ
い。
The plating solution purified by genus 4 was filtered and stored in an inert gas atmosphere. You can store it in the L tank.

この方法で建浴を連続的に行う装置としては、^IC1
,とBPCとの混合槽、金属^1による精製槽およびめ
っき液の貯蔵槽を密閉型にして、配管で順次接続してN
!l成する。そして、混合槽は、上部に不活性がス導入
排出口と計量した^IC1,やBPCを投入する投入口
とを設けておく。ここで、投入口は、不活性がス投人後
不活性ガスが漏れないように開閉型にしておく。また、
短時間に均一に混合できるようにするために攪袢機を、
さらに、発熱による危険を避けるために冷却器を取り付
けておく。
An example of a device that continuously prepares baths using this method is ^IC1.
, a mixing tank with BPC, a purification tank with metal ^1, and a storage tank for plating solution, which are sealed and connected sequentially with piping.
! I will make it. The mixing tank is provided with an inert gas inlet/outlet and an inlet for introducing the measured amount of IC1 or BPC at the upper part. Here, the inlet is of an open/close type so that the inert gas does not leak after the inert gas is poured. Also,
In order to mix uniformly in a short time, a stirrer is used.
Additionally, a cooler should be installed to avoid the risk of heat generation.

金属^1による精製槽、貯蔵槽も上部に不活性ガス導入
排出口を設け、前者には、常温で精製すると、通常数時
匍もかかるので、めっき液を加熱できるように加熱器を
取り付けておく。そして、これらの精製槽と貯蔵槽との
間の配管には、フィルターを設け、不溶物を除去する。
The purification tank and storage tank for metal^1 are also equipped with an inert gas inlet/outlet at the top, and the former is equipped with a heater to heat the plating solution, as refining at room temperature usually takes several hours. put. A filter is provided in the piping between the purification tank and the storage tank to remove insoluble matter.

上記各種間のめっき液移送は、めっき液のヘッドを利用
してもよく、ポンプによってもよい。なお、めっき液と
接触する各相の内面、付属機器および配管は、めっき液
が腐食性の強いものであるので、耐食材料(例えば、フ
ッ素樹脂、グラス7アイバー)で被覆しておき、フィル
ターも耐食材料製のものにする。
The plating solution may be transferred between the various types by using a plating solution head or by a pump. Since the plating solution is highly corrosive, the inner surfaces of each phase, auxiliary equipment, and piping that come into contact with the plating solution should be coated with a corrosion-resistant material (e.g., fluororesin, Glass 7 Ivar), and the filters should also be covered. It should be made of corrosion-resistant material.

(実施例) 第1図は、本発明の1実施例を示すもので、1は、^I
C1,とBPCとの混合槽である。この混合槽1は密閉
型で、上部にはバルブ2.2aを有する2個のホッパー
3.3aと不活性ガス導入排出口4とが設けられ、両ホ
ッパー3.3aの上部は、密閉型の薬品投入槽5に収容
されている。この薬品投入槽5には、図示してないが、
手袋を有する窓が設けられていて、密閉した状態で内部
作業ができるようになっており、内部には八1C1,と
IIIPCおよび計量器が入れられている。そして、上
部には不活性がス導入排出口4aが設けられている。
(Example) FIG. 1 shows an example of the present invention, where 1 is ^I
This is a mixing tank for C1 and BPC. This mixing tank 1 is a closed type, and the upper part is provided with two hoppers 3.3a having a valve 2.2a and an inert gas inlet/outlet 4. The upper part of both hoppers 3.3a is a closed type. It is housed in a chemical input tank 5. Although not shown in this chemical input tank 5,
A window with gloves is provided so that the interior can be worked on in a sealed manner, and the 81C1, IIIPC and measuring instrument are placed inside. An inert gas inlet/outlet 4a is provided at the upper part.

また、混合槽1には、Wt件磯6と温度計7とが内部に
取り付けられ、外周には冷却パイプ8が巡らされている
Further, a Wt rock 6 and a thermometer 7 are installed inside the mixing tank 1, and a cooling pipe 8 is arranged around the outer periphery.

混合槽1の下側には、バルブ2bを有する配管9により
開裂W110が接続されている。この精製f″[0は、
密閉型で、外周に加熱パイプ11が、また、上部に不活
性ガス導入排出口4bが設けられており、さらに、内部
に^I#!12が装入されている。
A cleavage W110 is connected to the lower side of the mixing tank 1 by a pipe 9 having a valve 2b. This refined f″[0 is
It is a closed type, and has a heating pipe 11 on the outer periphery, an inert gas inlet/outlet 4b at the top, and ^I#! inside. 12 are loaded.

精製槽10の側面および下側には、それぞれバルブ2c
、ろ過装置13およびポンプ14を有する配管9aおよ
びバルブ2dを有する配管9bがなされていて、配管9
aは、上部に不活性がス導入排出口4Cを有するめっき
液の貯蔵槽15に接続されている。
Valves 2c are installed on the side and lower sides of the purification tank 10, respectively.
, a pipe 9a having a filtration device 13 and a pump 14, and a pipe 9b having a valve 2d.
a is connected to a plating solution storage tank 15 having an inert gas inlet/outlet 4C at the top.

この装置により建浴するには、まず、各桁の不活性ガス
導入排出口4〜4cを開いて、不活性ガスを導入し、槽
内部の空気を不活性ガスで置換する。この状態でバルブ
2.2aを開いて、ホッパー3.3aから別個に八1e
t3とBPCとを混合槽1に投入し、投入後バルブ2.
2aを閉じる。
To prepare a bath using this device, first, the inert gas inlet/outlet ports 4 to 4c of each digit are opened, inert gas is introduced, and the air inside the tank is replaced with the inert gas. In this state, open valve 2.2a and separate 81e from hopper 3.3a.
t3 and BPC are put into the mixing tank 1, and after the addition, the valve 2.
Close 2a.

両薬品を混合槽1に投入したなら、撹拌8!!6で混合
する。この際、温度が者しく高くなるようであれば、冷
却パイプ8で冷却する。ΔIC1,とBI’Cとが溶融
したなら、バルブ2 +)を開いて、めっき液を精製槽
10に落下させ、バルブ2bを閉じる。
Once both chemicals are added to mixing tank 1, stir 8! ! Mix at step 6. At this time, if the temperature becomes significantly high, the cooling pipe 8 is used to cool it down. Once ΔIC1 and BI'C are melted, valve 2+) is opened to allow the plating solution to fall into purification tank 10, and valve 2b is closed.

精製槽10にめっき液が入ると、めっき液の不純物は、
^1線に置換析出し、めっき液は精製される。この精製
中にめっき液の温度が低下するようであれば、加熱パイ
プ11で加熱する。
When the plating solution enters the purification tank 10, impurities in the plating solution are
The plating solution is purified by displacement precipitation on the ^1 line. If the temperature of the plating solution decreases during this purification, it is heated with the heating pipe 11.

精製後は、バルブ2cを開いて、ポンプ14を作動させ
てろ過装置13でめっき液をろ過し、貯蔵槽15に移送
する。
After purification, the valve 2c is opened, the pump 14 is activated, the plating solution is filtered by the filtration device 13, and the plating solution is transferred to the storage tank 15.

この建浴装置でホッパー3.3aから^IcI、67モ
ル%とRPC33モル%とを投入して、めっき液を精!
!!WIioに100℃で10時間放置して精製し、そ
の精製めっき液で電気めっきしたところ、めっき層のへ
1純度は、従来の99.00%であったのに対して、9
9.97%であった。
In this bath preparation device, ^IcI, 67 mol% and RPC 33 mol% are charged from hopper 3.3a to prepare the plating solution!
! ! When purified by leaving it in WIio at 100°C for 10 hours and electroplating with the purified plating solution, the purity of the plating layer was 99.00%, compared to the conventional 99.00%.
It was 9.97%.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明法による建浴装置を示すものである。 1・・・混合槽、2.2a、 2b、 2e、 2d・
・・バルブ、3.3a−ホッパー、4.4a、4b14
cm不活性ガス導入排出口、5・・・薬品投入槽1.6
・・・攪袢機、7・・・温度計、8・・・冷却パイプ、
9.9a、9b、・・・配管、10・・・精製槽、11
・・・加熱パイプ、12・・・^I線、13・・・ろ過
装置、14・・・ポンプ、15・・・貯蔵槽、
FIG. 1 shows a bath preparation device according to the method of the present invention. 1... Mixing tank, 2.2a, 2b, 2e, 2d.
...Valve, 3.3a-Hopper, 4.4a, 4b14
cm Inert gas inlet/outlet, 5...Chemical input tank 1.6
... Stirrer, 7... Thermometer, 8... Cooling pipe,
9.9a, 9b...Piping, 10...Purification tank, 11
... Heating pipe, 12 ... ^I line, 13 ... Filtration device, 14 ... Pump, 15 ... Storage tank,

Claims (2)

【特許請求の範囲】[Claims] (1)塩化アルミニウムとブチルピリジニウムクロリド
とを不活性ガス雰囲気下で所定の比率で混合した後、同
雰囲気下で金属アルミニウムに接触させて置換反応によ
り不純物を除去し、しかる後にフィルターでろ過するこ
とを特徴とする非水溶液電気アルミニウムめっき浴の建
浴方法。
(1) After mixing aluminum chloride and butylpyridinium chloride in a predetermined ratio under an inert gas atmosphere, the mixture is brought into contact with metal aluminum under the same atmosphere to remove impurities through a substitution reaction, and then filtered. A method for preparing a non-aqueous electrolytic aluminum plating bath characterized by:
(2)攪袢機と冷却器とを備え、かつ、上部に開閉自在
な投入口が別個に設けられた混合槽と、加熱器を備え、
内部に金属アルミニウムが装入された精製槽とがバルブ
を有する配管により接続され、さらに、この精製槽とめ
っき液の貯蔵槽がろ過装置を有する配管で接続されてい
て、これらの各槽は、密閉型で、上部に不活性ガスの導
入排出口が設けられていることを特徴とする非水溶液電
気アルミニウムめっき浴の建浴装置。
(2) Equipped with a stirrer and a cooler, and a mixing tank with a separate input port that can be opened and closed at the top, and a heater,
A purification tank filled with metal aluminum is connected to the plating tank by a pipe having a valve, and this purification tank and a plating solution storage tank are connected by a pipe having a filtration device. A bath preparation device for a non-aqueous electrolytic aluminum plating bath, which is a closed type and is equipped with an inert gas inlet and outlet at the top.
JP62260493A 1987-10-15 1987-10-15 Building equipment for non-aqueous solution electric aluminum plating bath Expired - Lifetime JP2623482B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62260493A JP2623482B2 (en) 1987-10-15 1987-10-15 Building equipment for non-aqueous solution electric aluminum plating bath

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62260493A JP2623482B2 (en) 1987-10-15 1987-10-15 Building equipment for non-aqueous solution electric aluminum plating bath

Publications (2)

Publication Number Publication Date
JPH01104793A true JPH01104793A (en) 1989-04-21
JP2623482B2 JP2623482B2 (en) 1997-06-25

Family

ID=17348730

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62260493A Expired - Lifetime JP2623482B2 (en) 1987-10-15 1987-10-15 Building equipment for non-aqueous solution electric aluminum plating bath

Country Status (1)

Country Link
JP (1) JP2623482B2 (en)

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5244296A (en) * 1975-10-02 1977-04-07 Lion Corp Method of producing antimicrobial proteinaceous substance
JPS5773195A (en) * 1980-10-23 1982-05-07 Mitsui Alum Kogyo Kk Production of aluminum powder
JPS61243190A (en) * 1985-04-19 1986-10-29 Sumitomo Metal Ind Ltd Electroplating method with molten slat bath
JPS6270592A (en) * 1985-09-20 1987-04-01 Nisshin Steel Co Ltd Aluminum electroplating bath and plating method by said plating bath
JPS6270593A (en) * 1985-09-20 1987-04-01 Nisshin Steel Co Ltd Aluminum electroplating bath and plating method by said plating bath

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5244296A (en) * 1975-10-02 1977-04-07 Lion Corp Method of producing antimicrobial proteinaceous substance
JPS5773195A (en) * 1980-10-23 1982-05-07 Mitsui Alum Kogyo Kk Production of aluminum powder
JPS61243190A (en) * 1985-04-19 1986-10-29 Sumitomo Metal Ind Ltd Electroplating method with molten slat bath
JPS6270592A (en) * 1985-09-20 1987-04-01 Nisshin Steel Co Ltd Aluminum electroplating bath and plating method by said plating bath
JPS6270593A (en) * 1985-09-20 1987-04-01 Nisshin Steel Co Ltd Aluminum electroplating bath and plating method by said plating bath

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