JP2002173718A - Aluminum treatment method - Google Patents
Aluminum treatment methodInfo
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- JP2002173718A JP2002173718A JP2000371361A JP2000371361A JP2002173718A JP 2002173718 A JP2002173718 A JP 2002173718A JP 2000371361 A JP2000371361 A JP 2000371361A JP 2000371361 A JP2000371361 A JP 2000371361A JP 2002173718 A JP2002173718 A JP 2002173718A
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- JP
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- aluminum
- mass
- mass ppm
- ppm
- added
- 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.)
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Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、電解コンデンサ用、磁
気ディスク用に代表されるＴｉ、Ｖ、Ｚｒの含有量を低
濃度に制御する必要のあるアルミニウムまたはアルミニ
ウム合金に好適で、Ｔｉ，Ｖの含有量を低減し、Ｚｒ含
有量を制御した地金が得られるアルミニウムまたはアル
ミニウム合金の処理方法に関する。BACKGROUND OF THE INVENTION The present invention is suitable for aluminum or an aluminum alloy which needs to control the content of Ti, V and Zr at a low concentration, typically for electrolytic capacitors and magnetic disks. The present invention relates to a method for treating aluminum or an aluminum alloy, which can obtain a base metal having a reduced Zr content and a controlled Zr content.
【０００２】[0002]
【従来の技術】電解コンデンサ用、磁気ディスク等に使
用されるアルミニウム材料には、コンデンサの性能を維
持するため９９．９質量％以上の純度が要求され、Ｔ
ｉ，Ｖ，Ｚｒ、Ｂ等の不純物はそれぞれ１０ｐｐｍ以下
に規制されている。このような用途に適した高純度のア
ルミニウム材料を得るためには、まず、純度が９９．８
５重量％以上のアルミニウム地金又は電解精錬炉からの
溶湯を精製容器に移し、撹拌を伴った制御冷却条件下で
アルミニウム溶湯を冷却し、偏析凝固されたα−Ａｌ晶
を得ている。溶湯の冷却過程で、Ｓｉ，Ｆｅ，Ｍｎ等、
共晶系の不純物をアルミニウム溶湯から偏析分離でき
る。しかしながら、包晶系の元素である不純物Ｔｉ，
Ｖ、Ｚｒは製品側に濃縮されるので、これらの不純物を
偏析凝固法で除去するためには、偏析凝固法を実施する
前に予めＴｉ、Ｖ，Ｚｒを極力除去しておく必要があ
る。2. Description of the Related Art Aluminum materials used for electrolytic capacitors and magnetic disks are required to have a purity of 99.9% by mass or more in order to maintain the performance of the capacitors.
Impurities such as i, V, Zr, and B are each regulated to 10 ppm or less. In order to obtain a high-purity aluminum material suitable for such applications, first, the purity is 99.8.
5% by weight or more of the aluminum ingot or the molten metal from the electrolytic refining furnace is transferred to a purification vessel, and the molten aluminum is cooled under controlled cooling conditions with stirring to obtain segregated and solidified α-Al crystals. In the process of cooling the molten metal, Si, Fe, Mn, etc.
Eutectic impurities can be segregated and separated from molten aluminum. However, the impurities Ti, which are peritectic elements,
Since V and Zr are concentrated on the product side, in order to remove these impurities by the segregation solidification method, it is necessary to remove Ti, V, and Zr as much as possible before performing the segregation solidification method.
【０００３】従来、不純物としてＴｉ、Ｖ等の包晶系元
素をアルミニウム又はアルミニウム合金から除去する方
法としては、例えば次のような方法が開示されている。
アルミニウム溶湯に不純物として含有されているアルカ
リ金属元素を、フッ化アルミニウム（ＡｌＦ3）を添加
してフッ化物を形成させて除去する方法が、ＴＡＣ法と
して知られており、また、特開平７−２０７３６８号公
報では、不純物としてＴｉを含有するアルミニウム又は
アルミニウム合金溶湯中に、Ｃａ、Ｂａ、Ｍｇ、Ｍｎ、
Ｐｂの酸化物のいずれか一種以上の酸化物を添加し、不
純物Ｔｉとこれらの酸化物との複合酸化物を形成させて
これを分離することにより、アルミニウム又はアルミニ
ウム合金中のＴｉを除去している。さらに、不純物とし
て含有されているＴｉの２〜４倍の化学当量に相当する
Ｂを添加し、Ｔｉ−Ｂ化合物を生成させて除去する方法
も提案されている。Conventionally, the following method has been disclosed as a method for removing peritectic elements such as Ti and V from aluminum or aluminum alloys as impurities.
A method for removing an alkali metal element contained as an impurity in a molten aluminum by adding aluminum fluoride (AlF 3 ) to form a fluoride is known as a TAC method. No. 207368 discloses that Ca, Ba, Mg, Mn, and the like are contained in an aluminum or aluminum alloy melt containing Ti as an impurity.
By adding one or more oxides of Pb oxide, forming a compound oxide of impurity Ti and these oxides and separating the same, aluminum or aluminum alloy Ti is removed. I have. Furthermore, there has been proposed a method of adding B corresponding to 2 to 4 times the chemical equivalent of Ti contained as an impurity to generate and remove a Ti-B compound.
【０００４】[0004]
【発明が解決しようとする課題】Ｂを添加してＴｉ、
Ｖ、ＺｒをＴｉＢ2、ＶＢ2、ＺｒＢ2として除去する従
来の処理方法では、包晶系元素の合計化学当量に対しＢ
添加量を規定しているため、Ｂ添加量は原料中のＴｉ、
Ｖ、Ｚｒの初期濃度に依存する。包晶系元素の初期濃度
が低い場合、Ｂ添加量は少なくなる。一方、ＢとＴｉ、
Ｖ、Ｚｒとの反応性はＴｉ、Ｖ、Ｚｒに順に大きいた
め、Ｔｉ、Ｖ、Ｚｒの合計化学当量の２〜４倍に相当す
る量のＢを添加した際、Ｔｉ、ＶがＢによって十分に除
去できてもＺｒとは不十分な反応に終わってしまい、溶
湯中に１．０〜数質量ｐｐｍ残留する。しかもＢが未反
応のまま数十ｐｐｍ残留することとなる。SUMMARY OF THE INVENTION B is added to Ti,
In the conventional treatment method for removing V and Zr as TiB 2 , VB 2 and ZrB 2 , B is determined based on the total chemical equivalent of the peritectic element.
Since the amount of addition is specified, the amount of B added is Ti
It depends on the initial concentrations of V and Zr. When the initial concentration of the peritectic element is low, the amount of B added is small. On the other hand, B and Ti,
Since the reactivity with V and Zr is larger in the order of Ti, V and Zr, when B is added in an amount corresponding to 2 to 4 times the total chemical equivalent of Ti, V and Zr, Ti and V are sufficiently converted by B. Even if it can be removed, the reaction with Zr ends up being insufficient, leaving 1.0 to several ppm by mass in the molten metal. In addition, several tens ppm of B remains unreacted.
【０００５】電解コンデンサ、磁気ディスク等の品質特
性はアルミニウム中に含有される包晶系元素濃度に強く
影響される。最近、電解コンデンサに要求される品質特
性が強くなり、今までに開示されている処理方法では、
包晶系元素、特にＺｒの濃度を、要求される品質特性を
満たす濃度範囲にまで減少させることは困難になった。The quality characteristics of electrolytic capacitors, magnetic disks, and the like are strongly affected by the concentration of peritectic elements contained in aluminum. Recently, the quality characteristics required for electrolytic capacitors have become stronger, and in the processing methods disclosed so far,
It has become difficult to reduce the concentration of peritectic elements, especially Zr, to a concentration range that satisfies the required quality characteristics.
【０００６】[0006]
【課題を解決するための手段】本発明は、このような要
求に応えるべく案出されたものであり、偏析精製に先立
って、Ｔｉ、Ｖ、ＺｒとＢの反応を有効に使用し、Ｔ
ｉ、ＶのみならずＺｒをも低減させることのできるアル
ミニウム溶湯精製方法を提案するものである。DISCLOSURE OF THE INVENTION The present invention has been devised in order to meet such a demand, and has been proposed to effectively utilize the reaction of Ti, V, Zr and B with B prior to segregation purification.
An object of the present invention is to propose a method for purifying molten aluminum capable of reducing not only i and V but also Zr.
【０００７】本発明のアルミニウム精製方法は、その目
的を達成するため、不純物としてＴｉ、Ｖ、Ｚｒを含む
アルミニウム又はアルミニウム合金の溶湯へ、Ｔｉ
Ｂ2、ＶＢ2、ＺｒＢ2として計算される合計化学当量よ
りも更に１００〜２００質量ｐｐｍ多い量のＢを添加
し、未反応で溶湯中に存在するＢを１００〜２００質量
ｐｐｍに制御することによりＺｒを０．１〜１．０質量
ｐｐｍの濃度に制御するものである。次に、この工程が
終わったアルミニウムまたはアルミニウム合金溶湯へＴ
ｉ及び／又はＶを添加することによって、未反応で存在
する１００〜２００質量ｐｐｍのＢと反応させてＴｉＢ
2及び／又はＶＢ2を生成させ、Ｔｉ：１質量ｐｐｍ以
下，Ｖ：１質量ｐｐｍ以下，Ｚｒ：０．１〜１．０質量
ｐｐｍ、Ｂ：設定残留目標Ｂ濃度に制御する。さらに、
このような方法で処理されたアルミニウムまたはアルミ
ニウム合金の溶湯を偏析用原料として偏析精製し、Ｔ
ｉ：２質量ｐｐｍ以下，Ｖ：１質量ｐｐｍ以下，Ｚｒ：
０．１〜１．０質量ｐｐｍ以下、Ｂ：２質量ｐｐｍ以下
の高純度アルミニウムを得る。[0007] In order to achieve the object, the aluminum refining method of the present invention converts Ti or V alloy containing Ti, V or Zr into molten aluminum or aluminum alloy.
B is added in an amount of 100 to 200 mass ppm larger than the total chemical equivalent calculated as B 2 , VB 2 , and ZrB 2 to control the amount of unreacted B present in the molten metal to 100 to 200 mass ppm. Controls Zr to a concentration of 0.1 to 1.0 ppm by mass. Next, T is added to the aluminum or aluminum alloy melt after this process.
By adding i and / or V, TiB is reacted with 100 to 200 ppm by mass of B present unreacted.
2 and / or VB 2 are generated, and Ti is controlled to 1 mass ppm or less, V: 1 mass ppm or less, Zr: 0.1 to 1.0 mass ppm, and B: the set residual target B concentration. further,
The molten aluminum or aluminum alloy treated by such a method is purified by segregation as a raw material for segregation.
i: 2 mass ppm or less, V: 1 mass ppm or less, Zr:
High-purity aluminum of 0.1 to 1.0 mass ppm or less and B: 2 mass ppm or less is obtained.
【０００８】[0008]
【作用】本発明者等は、アルミニウム溶湯に含まれてい
るＴｉ，Ｖ，ＺｒとＢ等の相互反応を詳細に調査・研究
した。その結果、以下のような作用があることを見出し
た。Ｔｉ，Ｖ，Ｚｒを含むアルミニウム溶湯に、Ａｌ−
Ｂ母合金等としてＢを添加するとＴｉＢ2、ＶＢ2、Ｚｒ
Ｂ2の金属間化合物が生成し、溶湯中に懸濁または炉底
に沈殿する。この金属間化合物を工業的には、沈降分
離、浮上分離、フィルター分離等により、アルミニウム
溶湯中から分離する。しかし、ＴｉＢ2、ＶＢ2、ＺｒＢ
2として計算される合計化学当量と同量のＢを投入して
も、未反応のＴｉ，Ｖ，ＺｒおよびＢが残留し、一般的
に工業的に実施される介在物除去方法では除去すること
ができない。そのため、通常、ＴｉＢ2、ＶＢ2、ＺｒＢ
2として計算される合計化学当量の数倍に相当するＢを
過剰に投入していた。The present inventors have investigated and studied in detail the interaction between Ti, V, Zr and B contained in the molten aluminum. As a result, they have found the following effects. Al-Al is added to molten aluminum containing Ti, V, and Zr.
When B is added as a B master alloy or the like, TiB 2 , VB 2 , Zr
Intermetallic compounds B 2 is produced, precipitates suspended or furnace bottom into the molten metal. This intermetallic compound is industrially separated from the molten aluminum by sedimentation separation, flotation separation, filter separation, or the like. However, TiB 2 , VB 2 , ZrB
Even if B is added in the same amount as the total chemical equivalent calculated as 2 , unreacted Ti, V, Zr and B remain, and should be removed by an industrially practiced inclusion removal method. Can not. Therefore, usually, TiB 2 , VB 2 , ZrB
B corresponding to several times the total chemical equivalent calculated as 2 was excessively charged.
【０００９】一方、ＢとＴｉ，Ｖ，Ｚｒとの反応は、未
反応で存在するＢ濃度とＴｉ、Ｖ、Ｚｒとの平衡が成立
し、未反応のＢが多いほど未反応のＴｉ，Ｖ，Ｚｒはそ
れぞれ少なくなる。また未反応のＢが同一量の場合で
は、Ｔｉ，Ｖ，ＺｒはＴｉ，Ｖ，Ｚｒの順に低濃度で平
衡する。その結果、Ｔｉ，Ｖ，Ｚｒを同時に含有するア
ルミニウム溶湯中にＢを投入した場合、Ｚｒ，Ｖ，Ｔｉ
の順に未反応の元素が多く残留し、平衡する。On the other hand, in the reaction of B with Ti, V, and Zr, the equilibrium between the unreacted B concentration and Ti, V, and Zr is established, and the more unreacted B, the more unreacted Ti, V , Zr decrease. When the amount of unreacted B is the same, Ti, V, and Zr equilibrate at lower concentrations in the order of Ti, V, and Zr. As a result, when B is introduced into an aluminum melt containing Ti, V, and Zr at the same time, Zr, V, Ti
In this order, many unreacted elements remain and equilibrate.
【００１０】Ｔｉ，Ｖ，Ｚｒの初期濃度が低い場合、従
来、投入するＢ量がそれに応じて少なくなるため、未反
応のＢ濃度が小さくなり、それと平衡する未反応のＴ
ｉ，Ｖ，Ｚｒ濃度はそれに応じ大きくなる。更に、Ｔ
ｉ，Ｖ，Ｚｒの順に残留濃度が増加するため、Ｔｉ、Ｖ
が十分に除去できても、Ｚｒはそれと平衡する未反応の
Ｂが少なくなり、その結果、Ｚｒは溶湯中に１．０〜数
質量ｐｐｍ程度残留する。When the initial concentration of Ti, V, and Zr is low, the amount of B to be introduced is conventionally reduced accordingly, so that the concentration of unreacted B is reduced, and the unreacted T which is in equilibrium therewith.
The i, V, and Zr concentrations increase accordingly. Further, T
Since the residual concentration increases in the order of i, V, and Zr, Ti, V
Can be sufficiently removed, Zr has less unreacted B in equilibrium with it, and as a result, about 1.0 to several ppm by mass of Zr remains in the molten metal.
【００１１】これに対し，ＴｉＢ2、ＶＢ2、ＺｒＢ2と
して計算される合計化学当量に当たるＢ量に更に１００
〜２００質量ｐｐｍの範囲でＢを多く添加した場合、未
反応の形で残存するＴｉ，Ｖ、ＺｒとＢとが平衡し、未
反応で存在するＢはＴｉ，Ｖ，Ｚｒの初期濃度に関わら
ず、常に１００〜２００質量ｐｐｍの濃度で残存され
る。本発明では、１００〜２００質量ｐｐｍの未反応Ｂ
量と平衡する未反応のＴｉ、Ｖ、Ｚｒ濃度が未反応Ｂ濃
度に応じて一定になることを見出し、未反応のＢ濃度の
制御により、Ｔｉ，Ｖ，Ｚｒの中で最も多く残留して平
衡するＺｒにおいても、０．１〜１．０質量ｐｐｍの範
囲内に留まるようにすることができたものである。On the other hand, the B amount corresponding to the total chemical equivalent calculated as TiB 2 , VB 2 and ZrB 2 is further increased by 100.
When a large amount of B is added in the range of 200 ppm by mass, Ti, V, and Zr remaining in an unreacted form are equilibrated with B, and B present in the unreacted state depends on the initial concentration of Ti, V, and Zr. And always remain at a concentration of 100 to 200 ppm by mass. In the present invention, 100 to 200 ppm by mass of unreacted B
It has been found that the unreacted Ti, V, and Zr concentrations equilibrating with the amount become constant in accordance with the unreacted B concentration, and by controlling the unreacted B concentration, the most unreacted Ti, V, Zr remains. Even in the equilibrium Zr, it could be kept within the range of 0.1 to 1.0 ppm by mass.
【００１２】しかし、このままでは過剰の未反応Ｂを含
有することとなって、後工程の偏析精製処理を行っても
Ｂを十分に除去することはできない。そこで、未反応の
Ｂと化学当量のＴｉ及び／又はＶを添加して未反応のＢ
と反応させ、ＴｉＢ2及び／又はＶＢ2を生成させて除去
する。過剰のＢが含有されているアルミニウム溶湯にＡ
ｌ−Ｔｉ母合金等のＴｉ成分を添加すると、Ａｌ−Ｔｉ
母合金が溶解している周辺にＴｉリッチの溶湯部分で溶
湯中のＢと反応してＴｉＢ2を生成する。また、溶湯全
体にＴｉが拡散した状態でも、同様にＴｉＢ2が生成す
る。生成したＴｉＢ2は、溶湯中に懸濁し、または炉低
に沈降する。すなわち、Ｂを除去するＴｉ処理ではＴｉ
Ｂ2の化学当量で反応が進行することから、目標残留Ｂ
量を除く、除去反応Ｂ量に対する化学当量分のＴｉを添
加すればよい。However, as it is, the unreacted B is contained as it is, so that B cannot be sufficiently removed even if a segregation purification treatment in a subsequent step is performed. Therefore, unreacted B and unreacted B are added by adding a chemical equivalent of Ti and / or V.
To form and remove TiB 2 and / or VB 2 . A in aluminum melt containing excess B
When a Ti component such as an l-Ti master alloy is added, Al-Ti
The Ti-rich molten metal reacts with B in the molten metal in the vicinity where the mother alloy is melted to generate TiB 2 . Further, even when Ti is diffused throughout the molten metal, TiB 2 is similarly generated. The produced TiB 2 is suspended in the molten metal or settles in the furnace. That is, in the Ti treatment for removing B, Ti
Since the reaction proceeds at the chemical equivalent of B 2 , the target residual B
It suffices to add a chemical equivalent of Ti to the removal reaction B amount, excluding the amount.
【００１３】Ｖを利用する際も、同様に除去反応Ｂ量に
対する化学当量分のＶを添加すれば十分である。また、
実際の操業では、Ｔｉ或いはＶは残留させたくないの
で、残留Ｂ量の目標値として１０〜３０質量ｐｐｍを設
定し、残りの除去Ｂ量に対応するＴｉ又はＶを添加す
る。さらに、脱ＢにＴｉ，Ｖを利用する際、反応時間の
点で、Ｖを利用するよりもＴｉを利用する方が工業的に
は有利である。その結果、使用するアルミニウム又はア
ルミニウム合金に不純物として含まれる包晶系元素の初
期濃度に関わらずＴｉ、Ｖを１質量ｐｐｍ以下に低減
し、Ｚｒを０．１〜１．０質量ｐｐｍに制御する処理が
可能となる。When V is used, it is sufficient to add a chemical equivalent of V to the amount of the removal reaction B in the same manner. Also,
In actual operation, Ti or V is not desired to remain, so 10 to 30 ppm by mass is set as the target value of the residual B amount, and Ti or V corresponding to the remaining removed B amount is added. Furthermore, when using Ti and V for de-B, it is industrially more advantageous to use Ti than to use V in terms of reaction time. As a result, Ti and V are reduced to 1 mass ppm or less and Zr is controlled to 0.1 to 1.0 mass ppm irrespective of the initial concentration of the peritectic element contained as an impurity in the aluminum or aluminum alloy used. Processing becomes possible.
【００１４】なお、Ｂを添加しての脱Ｔｉ，Ｖ，Ｚｒ処
理及び脱Ｂ処理されるアルミニウム溶湯は、７００〜９
００℃の温度域に維持されることが好ましい。このとき
の溶湯温度が７００℃に達しないと、ＴｉＢ２ ，ＶＢ
２ の生成反応が遅くなり、生産性が低下する。ＴｉＢ
２ ，ＶＢ２ の生成反応は９００℃を超える溶湯温度で
も進行するが、過度に高い温度はエネルギ消費量が多く
なるばかりでなく、炉壁耐火物の溶損を促進させる。The aluminum melt to be subjected to Ti, V, Zr treatment and B treatment by adding B is 700 to 9%.
It is preferable to maintain the temperature range of 00 ° C. If the melt temperature at this time does not reach 700 ° C., TiB 2, VB
2 slows down the production reaction and lowers productivity. TiB
2, The formation reaction of VB2 proceeds even at a molten metal temperature exceeding 900 ° C., but an excessively high temperature not only increases the energy consumption but also promotes the erosion of the furnace wall refractory.
【００１５】[0015]
【実施の態様】本発明の実施の態様を添付の図面及び具
体的な例を参照しながら、説明する。図１は、本発明に
係るアルミニウム又はアルミニウム合金の処理装置の一
実施の態様の概略構成を示す模式的縦断面である。処理
装置は、図１に示すように、黒鉛、不定形耐火物又は耐
火レンガを内張りし、原料溶湯ＭＭを保持する保持容器
１と、この保持容器１中の原料溶湯ＭＭにＢを添加する
Ｂ添加装置２とＴｉ及び／又はＶを添加する添加装置３
と、生成するＴｉＢ2、ＶＢ2、ＺｒＢ2の金属間化合物
を浮上分離するための攪拌装置４とを備えている。ここ
で、ＢとはＡｌ−Ｂ合金、ＮａＢＦ4フラックス、ＫＢ
Ｆ4フラックス等のＢ含有物質のことを言い、Ｔｉ及び
／又はＶとはＡｌ−Ｔｉ母合金、Ａｌ−Ｖ母合金、Ｋ2
ＴｉＦ6フラックス等のＴｉ及び／又はＶ含有物質のこ
とを言い、特に添加物質種を限定するものではない。DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described with reference to the accompanying drawings and specific examples. FIG. 1 is a schematic longitudinal section showing a schematic configuration of an embodiment of an aluminum or aluminum alloy processing apparatus according to the present invention. As shown in FIG. 1, the processing apparatus includes a holding container 1 for holding raw material MM, which is lined with graphite, an amorphous refractory or a refractory brick, and adding B to the raw material MM in the holding container 1. Addition device 2 and addition device 3 for adding Ti and / or V
And a stirrer 4 for flotation-separating the generated intermetallic compounds of TiB 2 , VB 2 , and ZrB 2 . Here, B is Al-B alloy, NaBF 4 flux, KB
A B-containing substance such as F 4 flux, and Ti and / or V are Al-Ti master alloy, Al-V master alloy, K 2
Refers to a Ti and / or V-containing substance such as a TiF 6 flux, and does not particularly limit the type of added substance.
【００１６】次に、図１に示す処理装置を用いての処理
方法手順について、説明する。 アルミニウム又はアルミニウム合金の所定量の原料
溶湯ＭＭを保持容器１にいれる。 原料溶湯に含有されているＴｉ量、Ｖ量及びＺｒ量
を分析する。 Ｔｉ，Ｖ，Ｚｒを除去し未反応のＢを制御するた
め、分析結果に基づいて、ＴｉＢ2、ＶＢ2、ＺｒＢ2と
して計算される合計化学当量に更に１００〜２００ｐｐ
ｍのＢを追加し、Ｂ添加装置２によって添加する。 攪拌装置４によって、原料溶湯ＭＭを攪拌して反応
を促進し、生成した金属間化合物を滓とともに浮上分離
する。 原料溶湯ＭＭ中にＴｉ及び／又はＶを、Ｔｉ及び／
又はＶ添加装置３によって添加する。この時、原料溶湯
ＭＭに未反応で残留するＢが制御されているため、特に
分析の必要はない。 攪拌装置４によって原料溶湯ＭＭを攪拌して反応を
促進し、生成した金属間化合物を浮上分離する。 以
上の手順により、Ｔｉ，Ｖ，Ｚｒを低減したアルミニウ
ム溶湯を偏析精製し、高純度のアルミニウムを得る。Next, a procedure of a processing method using the processing apparatus shown in FIG. 1 will be described. A predetermined amount of raw material molten metal MM of aluminum or aluminum alloy is put in holding container 1. The amounts of Ti, V and Zr contained in the raw material melt are analyzed. In order to remove Ti, V, and Zr and control unreacted B, the total chemical equivalent calculated as TiB 2 , VB 2 , and ZrB 2 is further 100 to 200 pp based on the analysis result.
m of B is added and added by the B adding device 2. The raw material melt MM is stirred by the stirrer 4 to promote the reaction, and the generated intermetallic compound is floated and separated together with the slag. Ti and / or V in the raw molten metal MM, Ti and / or
Alternatively, it is added by the V addition device 3. At this time, since B remaining unreacted in the raw material melt MM is controlled, there is no particular need for analysis. The raw material melt MM is stirred by the stirrer 4 to promote the reaction, and the generated intermetallic compound is floated and separated. By the above procedure, the aluminum melt in which Ti, V, and Zr are reduced is purified by segregation to obtain high-purity aluminum.
【００１７】次に、この手順に沿って、アルミニウム溶
湯を処理した実例を紹介する。内径が８００ｍｍ、内部
高さが１０００ｍｍの処理装置の保持容器１中へ、溶湯
深さ８００ｍｍとなるように８００℃で溶解したアルミ
ニウム溶湯を入れた。アルミニウム溶湯をサンプリング
し、分析したところ、Ｔｉ：３０質量ｐｐｍ、Ｖ：５０
質量ｐｐｍ、Ｚｒ：６質量ｐｐｍであった。続いて、Ｔ
ｉＢ2、ＶＢ2、ＺｒＢ2として計算される合計化学当量
に更にＢを１２０質量ｐｐｍ追加されるように、Ａｌ−
Ｂ母合金を３．０ｋｇ添加した後、攪拌装置４による攪
拌羽根を４００ｒｐｍで回転させ１０分間攪拌した。生
成した金属間化合物を浮上分離した後の溶湯を分析した
ところ、Ｔｉ：０．４質量ｐｐｍ、Ｖ：０．６質量ｐｐ
ｍ、Ｚｒ：０．８質量ｐｐｍ、Ｂ：１１８質量ｐｐｍを
含むアルミニウム溶湯であった。Next, an example in which the molten aluminum is treated according to this procedure will be introduced. A molten aluminum melted at 800 ° C. was placed in a holding vessel 1 of a processing apparatus having an inner diameter of 800 mm and an inner height of 1000 mm so as to have a molten metal depth of 800 mm. When the aluminum melt was sampled and analyzed, Ti: 30 mass ppm, V: 50
Ppm by mass, Zr: 6 ppm by mass. Then, T
Al- is added so that 120 mass ppm of B is added to the total chemical equivalent calculated as iB 2 , VB 2 , and ZrB 2 .
After adding 3.0 kg of the B master alloy, the stirring blade of the stirring device 4 was rotated at 400 rpm and stirred for 10 minutes. Analysis of the molten metal after flotation separation of the generated intermetallic compound revealed that Ti: 0.4 mass ppm and V: 0.6 mass pp.
The molten aluminum contained m, Zr: 0.8 mass ppm, and B: 118 mass ppm.
【００１８】比較のために前記と同条件で、ＴｉＢ2、
ＶＢ2、ＺｒＢ2として計算される合計化学当量の２倍に
当たるＢに相当するよう、Ａｌ―Ｂ合金を１．３ｋｇ添
加した。その結果、アルミニウム溶湯は、Ｔｉ：０．８
質量ｐｐｍ、Ｖ：１．０質量ｐｐｍ、Ｚｒ：２．１質量
ｐｐｍ、Ｂ：３５質量ｐｐｍを含有するものになってい
た。For comparison, TiB 2 ,
1.3 kg of an Al-B alloy was added so as to correspond to B corresponding to twice the total chemical equivalent calculated as VB 2 and ZrB 2 . As a result, the molten aluminum becomes Ti: 0.8
It contained ppm by mass, V: 1.0 ppm by mass, Zr: 2.1 ppm by mass, and B: 35 ppm by mass.
【００１９】次に、未反応のＢを過剰に残留させている
アルミニウム溶湯の脱Ｂ処理の状況を説明する。前記方
法で得られたＴｉ：０．４質量ｐｐｍ、Ｖ：０．６質量
ｐｐｍ、Ｚｒ：０．８質量ｐｐｍ、Ｂ：１１８質量ｐｐ
ｍを含むアルミニウム溶湯中へ、残留目標Ｂ量を１２ｐ
ｐｍとして、反応対象Ｂ量に対してＴｉＢ2として計算
される化学当量のＴｉとしてＡｌ−Ｔｉ母合金を２．２
ｋｇ添加した。攪拌装置４による攪拌羽根を４００ｒｐ
ｍで回転させ１０分間攪拌した。その結果、Ｔｉ：０．
８質量ｐｐｍ、Ｖ：０．６質量ｐｐｍ、Ｚｒ：０．８質
量ｐｐｍ、Ｂ：１２質量ｐｐｍを含むアルミニウム溶湯
が得られた。Next, the situation of the de-B treatment of the molten aluminum in which unreacted B is excessively remaining will be described. Ti obtained by the above method: 0.4 mass ppm, V: 0.6 mass ppm, Zr: 0.8 mass ppm, B: 118 mass pp
12p into the molten aluminum containing m
As an equivalent Ti calculated as TiB 2 with respect to the amount of B to be reacted as pm, an Al-Ti master alloy is 2.2.
kg was added. 400 rpm of the stirring blade by the stirring device 4
and stirred for 10 minutes. As a result, Ti: 0.
An aluminum melt containing 8 mass ppm, V: 0.6 mass ppm, Zr: 0.8 mass ppm, and B: 12 mass ppm was obtained.
【００２０】この溶湯を、特公昭６１−３６５６８号公
報に記載の方法にしたがって偏析精製した。得られた精
製地金は、Ｔｉ：０．９質量ｐｐｍ、Ｖ：１．０質量ｐ
ｐｍ、Ｚｒ：０．９質量ｐｐｍ、Ｂ：１質量ｐｐｍでア
ルミニウム純度が９９．９質量％以上となっており、電
解コンデンサ用材料、磁気ディスク用材料として十分に
使用可能な地金であった。精製地金を取り出した残りの
溶湯地金は、Ｔｉ、Ｖ、Ｚｒ、Ｂとも従来の品質特性要
求でＢ処理していた場合と変わらない濃度なので、用途
の制約を受けることはない。This molten metal was purified by segregation according to the method described in JP-B-61-36568. The obtained refined metal was Ti: 0.9 mass ppm, V: 1.0 mass p
The aluminum purity was 99.9% by mass or more at pm, Zr: 0.9% by mass, and B: 1% by mass, and the metal was sufficiently usable as a material for electrolytic capacitors and a material for magnetic disks. . The remaining molten metal from which the refined metal has been taken out has the same concentration as that of the case where B processing has been performed in accordance with the conventional quality characteristic requirements for Ti, V, Zr, and B, and thus there is no restriction on applications.
【００２１】[0021]
【発明の効果】以上に説明したように、本発明のアルミ
ニウム処理方法では、使用するアルミニウム又はアルミ
ニウム合金のＴｉ、Ｖ，Ｚｒ初期濃度に関わらず、溶湯
中のＴｉ、Ｖ，Ｚｒに対して合計化学当量よりも適宜過
剰のＢを添加して、ＴｉＢ2、ＶＢ2、ＺｒＢ2を生成さ
せて除去し、溶湯中に未反応のＢを残留させてＺｒをも
１．０質量ｐｐｍ以下に低減し、その後未反応のＢをＴ
ｉ及び／又はＶの添加でＴｉＢ2、ＶＢ2の形にして除去
できるので、その後の偏析精製法と相俟って、高純度の
アルミニウム又はアルミニウム合金を得ることができ、
電解コンデンサ用、磁気ディスク用に適した素材を提供
することができる。As described above, in the aluminum treatment method of the present invention, the total amount of Ti, V, and Zr in the molten metal is independent of the initial concentration of Ti, V, and Zr of the aluminum or aluminum alloy used. An appropriate excess of B than the chemical equivalent is added to generate and remove TiB 2 , VB 2 , and ZrB 2, and unreacted B remains in the molten metal to reduce Zr to 1.0 mass ppm or less. Then, unreacted B is replaced with T
Since it can be removed in the form of TiB 2 or VB 2 by adding i and / or V, high purity aluminum or aluminum alloy can be obtained in combination with the subsequent segregation purification method,
A material suitable for an electrolytic capacitor and a magnetic disk can be provided.
【図１】 本発明において使用するアルミニウム処理装
置のの概要を示す概念図である。FIG. 1 is a conceptual diagram showing an outline of an aluminum processing apparatus used in the present invention.
１； 保持容器 ２； Ｂ添加装置 ３； Ｔｉ及び／又はＶ添加装置 ４； 攪拌装置 ＭＭ； 原料溶湯 DESCRIPTION OF SYMBOLS 1; Holding container 2; B addition device 3; Ti and / or V addition device 4; Stirring device MM;
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２２Ｃ 21/00 Ｃ２２Ｃ 21/00 Ｎ ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) C22C 21/00 C22C 21/00 N
Claims (4)
ミニウム又はアルミニウム合金の溶湯へ、ＴｉＢ2、Ｖ
Ｂ2、ＺｒＢ2として計算される合計化学当量よりも更に
１００〜２００質量ｐｐｍ多い量のＢを添加し、未反応
で溶湯中に存在するＢを１００〜２００質量ｐｐｍに制
御することによりＺｒを０．１〜１．０質量ｐｐｍの濃
度に制御することを特徴とするアルミニウムまたはアル
ミニウム合金の処理方法。1. TiB 2 and V are added to a molten aluminum or aluminum alloy containing Ti, V and Zr as impurities.
B 2 , Zr is added by adding an amount of B that is 100 to 200 mass ppm larger than the total chemical equivalent calculated as ZrB 2 and controlling unreacted B present in the molten metal to 100 to 200 mass ppm. A method for treating aluminum or an aluminum alloy, wherein the concentration is controlled to 0.1 to 1.0 ppm by mass.
ニウムまたはアルミニウム合金溶湯へ、設定残留目標を
除く、未反応Ｂ量に対応するＴｉ及び／又はＶの化学当
量を添加することによって、未反応で存在する１００〜
２００質量ｐｐｍのＢと反応させて、ＴｉＢ2及び／又
はＶＢ2を生成させ、Ｔｉ：１質量ｐｐｍ以下，Ｖ：１
質量ｐｐｍ以下，Ｚｒ：０．１〜１．０質量ｐｐｍ、
Ｂ：設定残留目標Ｂ濃度に制御することを特徴とするア
ルミニウムまたはアルミニウム合金の処理方法。2. The method according to claim 1, wherein a chemical equivalent of Ti and / or V corresponding to the unreacted B amount is added to the molten aluminum or aluminum alloy, excluding the set residual target. 100 to 100 present in the reaction
By reacting with 200 mass ppm of B to form TiB 2 and / or VB 2 , Ti: 1 mass ppm or less, V: 1
Mass ppm or less, Zr: 0.1 to 1.0 mass ppm,
B: A method for treating aluminum or an aluminum alloy, which is controlled to a set residual target B concentration.
理されたアルミニウムまたはアルミニウム合金の溶湯を
原料として偏析精製するアルミニウムまたはアルミニウ
ム合金の処理方法。3. A method for treating aluminum or an aluminum alloy, wherein the molten aluminum or aluminum alloy treated according to claim 1 or 2 is used as a raw material for segregation purification.
ｐｍ以下，Ｖ：１質量ｐｐｍ以下，Ｚｒ：０．１〜１．
０質量ｐｐｍ以下、Ｂ：２質量ｐｐｍ以下である請求項
３に記載のアルミニウムまたはアルミニウム合金の処理
方法。4. The segregated and refined metal is Ti: 2 mass p
pm or less, V: 1 mass ppm or less, Zr: 0.1-1.
The method for treating aluminum or an aluminum alloy according to claim 3, wherein the content is 0 mass ppm or less and B: 2 mass ppm or less.
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|---|---|---|---|
| JP2000371361A JP3458840B2 (en) | 2000-12-06 | 2000-12-06 | Aluminum processing method |
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|---|---|---|---|
| JP2000371361A JP3458840B2 (en) | 2000-12-06 | 2000-12-06 | Aluminum processing method |
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| JP3458840B2 JP3458840B2 (en) | 2003-10-20 |
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| JP2009280918A (en) * | 2003-03-18 | 2009-12-03 | Showa Denko Kk | Method for refining aluminum, high purity aluminum material, method for producing aluminum material for electrode of electrolytic capacitor and aluminum material for electrode of electrolytic capacitor |
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