JPH0422977B2 - - Google Patents
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- Publication number
- JPH0422977B2 JPH0422977B2 JP62047807A JP4780787A JPH0422977B2 JP H0422977 B2 JPH0422977 B2 JP H0422977B2 JP 62047807 A JP62047807 A JP 62047807A JP 4780787 A JP4780787 A JP 4780787A JP H0422977 B2 JPH0422977 B2 JP H0422977B2
- Authority
- JP
- Japan
- Prior art keywords
- filtration
- filter
- aluminum
- inclusions
- pressure
- 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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Classifications
-
- 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)
Description
産業上の利用分野
本発明は、アルミニウムまたはアルミニウム合
金（以下、両者を併せて単にアルミニウムとい
う）溶湯中に含まれる介在物の濾過方法に関する
ものである。
従来の技術
近年、アルミニウム製品の高品質化の要求の伴
い、鋳塊の溶解鋳造における溶湯処理の品質管
理、時に溶湯中の介在物の管理については、その
重要性が強く認識されてきている。この背景に
は、電子機器などの先端技術分野へのアルミニウ
ム材料の適用範囲が拡大されてきたことと、磁気
デイスク材、スパツターターゲツト材、ボンデイ
ングワイヤー、箔地に代表されるように、製品の
薄肉化および表面の加工精度などが著しく進んで
きたことがある。従つて、従来では全く問題視さ
れなかつた微小介在物や晶出物の大きさが、製品
欠陥に直接結び付くようになり、磁気デイスクメ
デイアの性能欠陥、スパツター性能の劣化、伸線
破断等のトラブルとして現れるので、高品質素材
への要求は一段と厳しいものとなつてきている。
溶融アルミニウムを濾過する濾過機としては、
フイルターに米国特許第3524548号又は特開昭52
−22327号に提案されているようなセラミツク製
の多孔質体を使用する例が多い。またのそ介在物
除去性能に着目すると、従来の濾過機の中では最
も微細なものまで除去する。
しかし、前記濾過機は、濾過機の入湯と出湯の
湯面のレベル差に基づくメタルヘツド差を利用し
て濾過する機構であるので、フイルターの気孔径
は通常200μｍ以上であつて、使用開始時の抵抗
が高くなることから、これより細かい孔径とする
ことは不可能である。また、この場合の濾過状況
を顕微鏡観察すると、非金属介在物は凝集フロツ
クとして存在し、フイルター孔にブリツジを形成
し、そのケーキ層によつて濾過が行われるため、
現実には孔径より遥かに細かな粒子まで捕捉され
ている。しかし、介在物除去効率を高めるため濾
過速度を最小にして運転しても、その外在物除去
効率は、溶湯不溶性微細TiB2をアルミニウム溶
湯の介在物として添加して濾過し、濾過された溶
湯中の酸不溶性Tiを化学分析して求めた結果、
従来の濾過効率は第１図Ｂに示すように50％以下
であつた。
発明が解決しようとする問題点
本発明は、前記従来濾過機での介在物捕捉粒子
よりさらに微細な、従来方法では除去が困難であ
つた細かな粒径の介在物（単粒子径として2μｍ
以下）をも捕捉し、高い介在物除去効率を達成す
る濾過方法を提供するものである。
問題点を解決するための手段
かくして、本発明によれば、アルミニウムまた
はアルミニウム合金を濾過する方法において、平
均気孔径が10〜50μｍであるフイルターを使用
し、フイルター部での濾過速度が0.05〜0.8cm／
secとなるように加圧濾過することを特徴とする
アルミニウム溶湯の濾過方法が提供される。
即ち、従来の溶湯の重力濾過の代わりに、遥か
に微細平均孔径のフイルターを用いて加圧濾過す
ることにより、微細介在物の除去を行なうもので
ある。
本発明における濾過の機構は濾過後のフイルタ
ーを観察した結果、フイルター表面に介在物をト
ラツプする表面濾過主体の濾過機構である。
発明者らは、アルミニウム溶湯にTiB2ハード
ナーを添加し、溶湯中のTiB2微細粒子を介在物
の指標とし、平均孔径の異なるフイルターを用
い、溶湯の加圧濾過速度とTiB2除去率の関係を
調べ、第１図曲線Ａの如き関係を得た。この結果
等を考慮し、フイルターの平均気孔径は、10〜
50μｍ、好ましくは10〜30μｍの範囲であつて、
10μｍ未満では濾過抵抗が大となり現実的に使用
不適当で、また50μｍを超える場合は微小介在物
が漏出し易く介在物の除去効率が低下する。この
ような気孔径を有するフイルターを使用し、アル
ゴンガス等の不活性ガスの加圧下で溶湯が通過す
る実用最小濾過速度範囲で濾過することにより微
小介在物をトラツプするプレコート層が濾層に形
成され、微小介在物の除去効果を著しく改善する
ことができる。濾過速度としては、0.05〜0.8
cm／sec、好ましくは、0.05〜0.3cm／secの範囲
で、0.05cm／sec未満では、濾過時間が長くなり
実用的でなく、また、加圧圧力を増し、濾過速度
が0.8cm／secを超えると形成されたプレコート層
が破れる恐れがあり、微小介在物の除去効率が低
下し好ましくなく、上記範囲の濾過速度となるよ
うに加圧圧力を調整する。
なお、フイルターとしては、Al2O3、SiC、
Si3N4等を主成分とするセラミツク材料を骨材と
したものが好適に使用される。
更にアルミニウム−マグネシウム合金系へ
TiB2を添加した溶湯の場合、より良好な介在物
除去効率を得たが、これはMgOあるいはスピネ
ルとTiB2の凝集フロツク化が促進されるためと
解釈される。
ここに示した濾過圧及び濾過速度はアルニウム
及びアルミニウム合金地金を通常の溶製法で前処
理した溶湯についての値であり、特殊な溶湯（例
えば介在物を大量に含むもの）は、この限りでな
い。
本発明の後述する実施例で使用したアルミニウ
ム溶湯濾過装置の概念図を第２図の縦断面図に示
す。るつぼ２は装置本体１内に配置され、電熱コ
イル３によりるつぼ内に投入した供試材を溶融し
て、約720℃の温度に保持する。本装置例では濾
過後の溶湯をアルゴガス等の不活性ガスを供給
し、ルツボ同様電熱コイルで加熱した樋７を介し
て次の装置に供給するものであるが、濾過溶湯を
直接黒鉛るつぼ等に不活性ガス雰囲気下で受け取
ることもできる。
濾過処理に際しては、加圧蓋４を閉じて導管５
からアルゴンガス等の加圧気体をるつぼ７の溶湯
上面空間に導き、この加圧により溶湯をるつぼ底
部に設けた所定のフイルター６に通し、前記樋を
介して黒鉛るつぼで受け取り、冷却固化するもの
である。
本濾過装置に関しては、るつぼ内のメタルレベ
ル検出、または濾過メタル量を計量し、アルゴン
ガス等による加圧を停止し、再び注湯し、加圧す
るように、操作を全て自動化することも可能であ
る。また、装置本体１及びるつぼ２をフイルター
部６で二分割し、フイルターの交換を容易にする
こともできる。
実施例
以下、実施例により本発明をさらに具体的に説
明する。
実施例 １
99.997％AlにTiB2ハードナー（５％Ti＋１％
Ｂ＋残Al）を0.1％添加した地金20Kgを730℃で、
第２図に示す濾過装置の上部るつぼ内でアルゴン
雰囲気中で溶解した。溶解後、Cl2ガスで脱ガス
処理し、710±５℃で、1.0時間鎮静した。続いて
直径100mm、厚さ15mm、平均気孔径21μｍのアル
ミナを骨材としたアイコー(株)製フイルターを使用
し、濾過圧1.0Kg／cm2（濾過速度0.16cm／sec）で
アルゴンガスにより加圧濾過した。濾過溶湯を樋
下流に設けた黒鉛るつぼにアルゴンガス雰囲気下
で受け取り冷却固化した。酸不溶性Tiを化学分
析した結果、濾過前は8.4ppm、濾過後は1.0ppm
で介在物除去効率88.1％が得られた。
TiB2ハードナーに使用したTiB2の粒度分布は
測定の結果、次の第１表に示すとおりで、2μｍ
未満が98.7％を占めており、本発明濾過方法では
2μｍ以下の微細外在物を大部分除去しているこ
とが判る。
INDUSTRIAL APPLICATION FIELD The present invention relates to a method for filtering inclusions contained in molten aluminum or aluminum alloy (hereinafter both are simply referred to as aluminum). BACKGROUND OF THE INVENTION In recent years, with the demand for higher quality aluminum products, the importance of quality control of molten metal processing during melting and casting of ingots, and sometimes of inclusions in the molten metal, has been strongly recognized. The background to this is that the scope of application of aluminum materials to advanced technology fields such as electronic equipment has expanded, and that products such as magnetic disk materials, sputter target materials, bonding wires, and foil materials are becoming increasingly popular. There have been significant advances in thinning walls and surface processing accuracy. Therefore, the size of microscopic inclusions and crystallized substances, which were not seen as a problem in the past, are now directly linked to product defects, leading to problems such as performance defects in magnetic disk media, deterioration of sputtering performance, and wire breakage. As a result, the requirements for high-quality materials are becoming even more stringent. As a filter for filtering molten aluminum,
U.S. Patent No. 3524548 or Japanese Patent Application Laid-open No. 1983
There are many examples of using ceramic porous bodies as proposed in No. 22327. In terms of inclusion removal performance, it removes even the finest particles among conventional filters. However, since the above-mentioned filter uses a metal head difference based on the level difference between the hot water entering and exiting the filter, the pore diameter of the filter is usually 200 μm or more, and the pore size at the beginning of use is It is impossible to make the pore diameter smaller than this because the resistance will be high. In addition, when observing the filtration situation in this case with a microscope, the nonmetallic inclusions exist as aggregated flocs, forming bridges in the filter holes, and filtration is performed by the cake layer.
In reality, particles much smaller than the pore size are captured. However, even if the operation is performed with the filtration speed set to the minimum in order to increase the inclusion removal efficiency, the foreign substance removal efficiency is reduced by adding molten metal insoluble fine TiB 2 as an inclusion to the molten aluminum and filtering it. As a result of chemical analysis of acid-insoluble Ti in
Conventional filtration efficiency was less than 50%, as shown in Figure 1B. Problems to be Solved by the Invention The present invention solves the problem of inclusions that are even finer than the inclusion-capturing particles in the conventional filter, and which are difficult to remove with conventional methods (with a single particle diameter of 2 μm).
The purpose of the present invention is to provide a filtration method that also captures the following) and achieves high inclusion removal efficiency. Means for Solving the Problems Thus, according to the present invention, in a method for filtering aluminum or aluminum alloy, a filter having an average pore diameter of 10 to 50 μm is used, and the filtration rate in the filter portion is 0.05 to 0.8 μm. cm/
Provided is a method for filtering molten aluminum, which is characterized by filtering under pressure so that sec. That is, instead of the conventional gravity filtration of molten metal, fine inclusions are removed by pressure filtration using a filter with a much finer average pore diameter. As a result of observing the filter after filtration, the filtration mechanism in the present invention is a filtration mechanism mainly based on surface filtration that traps inclusions on the surface of the filter. The inventors added TiB 2 hardener to molten aluminum, used fine TiB 2 particles in the molten metal as an indicator of inclusions, and used filters with different average pore sizes to investigate the relationship between pressure filtration rate of molten metal and TiB 2 removal rate. was investigated, and a relationship such as curve A in Figure 1 was obtained. Considering this result etc., the average pore diameter of the filter is 10~
50 μm, preferably in the range of 10 to 30 μm,
If it is less than 10 μm, the filtration resistance becomes large and it is practically unsuitable for use, and if it exceeds 50 μm, minute inclusions tend to leak out and the removal efficiency of inclusions decreases. Using a filter with such a pore size, a pre-coat layer is formed on the filter layer that traps minute inclusions by filtering at the minimum practical filtration speed range at which the molten metal passes under the pressure of an inert gas such as argon gas. The removal effect of micro inclusions can be significantly improved. The filtration rate is 0.05-0.8
cm/sec, preferably in the range of 0.05 to 0.3 cm/sec; if it is less than 0.05 cm/sec, the filtration time becomes longer and is not practical; If it exceeds the filtration rate, there is a risk that the precoat layer formed will be torn, and the removal efficiency of minute inclusions will decrease, which is undesirable. In addition, as a filter, Al 2 O 3 , SiC,
A ceramic material whose main component is Si 3 N 4 or the like as an aggregate is preferably used. Furthermore, to aluminum-magnesium alloy system
In the case of the molten metal with TiB 2 added, better inclusion removal efficiency was obtained, which is interpreted to be due to the promotion of aggregation of MgO or spinel and TiB 2 into flocs. The filtration pressure and filtration speed shown here are values for molten metal pretreated with aluminum and aluminum alloy ingots using normal melting methods, and do not apply to special molten metals (for example, those containing a large amount of inclusions). . A conceptual diagram of a molten aluminum filtration device used in the later-described examples of the present invention is shown in the vertical cross-sectional view of FIG. The crucible 2 is disposed within the main body 1 of the apparatus, and the test material introduced into the crucible is melted by the electric heating coil 3 and maintained at a temperature of about 720°C. In this device example, the molten metal after filtration is supplied with an inert gas such as Argo gas, and is supplied to the next device via the gutter 7 heated by an electric heating coil like the crucible, but the filtered molten metal is directly transferred to a graphite crucible, etc. It can also be received under an inert gas atmosphere. During the filtration process, the pressure lid 4 is closed and the conduit 5 is
A pressurized gas such as argon gas is introduced into the space above the molten metal in the crucible 7, and the molten metal is passed through a predetermined filter 6 provided at the bottom of the crucible through the gutter, and is cooled and solidified. It is. Regarding this filtration device, it is also possible to automate all operations such as detecting the metal level in the crucible or measuring the amount of filtered metal, stopping pressurization with argon gas, etc., pouring the metal again, and applying pressure. be. Furthermore, the apparatus main body 1 and the crucible 2 can be divided into two by the filter section 6 to facilitate filter replacement. Examples Hereinafter, the present invention will be explained in more detail with reference to Examples. Example 1 99.997% Al with TiB 2 hardener (5% Ti + 1%
20 kg of metal with 0.1% of B + residual Al added at 730℃,
The solution was dissolved in an argon atmosphere in the upper crucible of the filtration apparatus shown in FIG. After dissolution, the mixture was degassed with Cl 2 gas and kept at 710±5°C for 1.0 hour. Next, a filter made by Aiko Co., Ltd. made of alumina aggregate with a diameter of 100 mm, a thickness of 15 mm, and an average pore size of 21 μm was used, and the filter was heated with argon gas at a filtration pressure of 1.0 Kg/cm 2 (filtration speed of 0.16 cm/sec). It was pressure filtered. The filtered molten metal was received in a graphite crucible placed downstream of the gutter under an argon gas atmosphere, and cooled and solidified. As a result of chemical analysis of acid-insoluble Ti, it was 8.4ppm before filtration and 1.0ppm after filtration.
An inclusion removal efficiency of 88.1% was obtained. The particle size distribution of TiB 2 used in TiB 2 hardener was measured as shown in Table 1 below, and was 2 μm.
In the filtration method of the present invention, 98.7% of the cases are less than
It can be seen that most of the fine external matter of 2 μm or less is removed.
【表】
また、上記と同様の操作を濾過圧2.0Kg／cm2
（濾過速度0.24cm／sec）で実施した場合の酸不溶
性Tiは濾過前7.5ppmに対し、濾過後1.3ppmであ
り、介在物除去効率は82.7％であつた。
実施例 ２
実施例１と同様の濾過操作を平均気孔径45μｍ
のフイルターで行なつた。濾過圧0.2Kg／cm2（濾
過速度0.12cm／sec）で酸不溶性Tiは濾過前
7.7ppm、濾過後3.6ppmであり、介在物除去前
7.7ppm、濾過後3.6ppmであり、介在物除去効率
は53.3％であつた。
実施例 ３
99.9％AlにTiB2ハードナー（５％Ti＋0.17B＋
残Al）を0.6％添加した溶湯10tを東京高級瀘材(株)
製のセラミチク製多孔質体のポーラス・チユーブ
フイルターで濾過後、DC鋳造した。
スラブサンプル10Kgを実施例１と同様、アルゴ
ン雰囲気下、720℃±５℃で溶製し、21μｍフイ
ルターを使用し、濾過圧1.0Kg／cm2（濾過速度
0.09cm／sec）で加圧濾過した。酸不溶性Tiは濾
過前3.6ppm、濾過後0.1ppmであり、介在物除去
効率は97.2％が得られた。
実施例 ４
Al−４％Mg合金（Mg4.06％、Si0.005％、
Fe0.001％、Cu0.0013％）にTiB2ハードナー（５
％Ti＋１％Ｂ＋残Al）を0.1％添加した地金10Kg
を、実施例１と同様アルゴン雰囲気下、710±５
℃で溶製し、平均気孔径45μｍのフイルターでア
ルゴン加圧下で濾過圧（濾過速度）を所定範囲内
で種々変更し濾過した。結果を第２表に示す。
第２表から判るように、高い介在物除去効率が
示される。[Table] Also, perform the same operation as above at a filtration pressure of 2.0Kg/cm 2
(filtration rate of 0.24 cm/sec), acid-insoluble Ti was 7.5 ppm before filtration and 1.3 ppm after filtration, and the inclusion removal efficiency was 82.7%. Example 2 The same filtration operation as in Example 1 was carried out using an average pore size of 45 μm.
This was done using a filter. Acid-insoluble Ti was removed before filtration at a filtration pressure of 0.2Kg/cm 2 (filtration speed 0.12cm/sec).
7.7ppm, 3.6ppm after filtration, before inclusion removal
It was 7.7 ppm, and 3.6 ppm after filtration, and the inclusion removal efficiency was 53.3%. Example 3 99.9% Al with TiB 2 hardener (5% Ti + 0.17B +
10 tons of molten metal with 0.6% residual aluminum added was sent to Tokyo Gyokugyoku Firozai Co., Ltd.
After filtration with a porous tube filter made of a ceramic material manufactured by Co., Ltd., it was cast by DC casting. As in Example 1, 10 kg of slab sample was melted at 720°C ± 5°C under an argon atmosphere, using a 21 μm filter, and with a filtration pressure of 1.0 kg/cm 2 (filtration rate
0.09cm/sec). Acid-insoluble Ti was 3.6 ppm before filtration and 0.1 ppm after filtration, and the inclusion removal efficiency was 97.2%. Example 4 Al-4%Mg alloy (Mg4.06%, Si0.005%,
Fe0.001%, Cu0.0013%) and TiB 2 hardener (5
10Kg of metal with 0.1% addition of %Ti + 1%B + balance Al)
710±5 under argon atmosphere as in Example 1.
The solution was prepared at 0.degree. C. and filtered under argon pressure using a filter having an average pore diameter of 45 .mu.m while varying the filtration pressure (filtration rate) within a predetermined range. The results are shown in Table 2. As can be seen from Table 2, high inclusion removal efficiency is shown.
【表】
発明の効果
本発明によれば、アルミニウム溶湯の濾過に、
従来試みられなかつた微細気孔径のフイルターを
用い加圧濾過することにより、アルミニウム中の
微細な介在物を高い除去効率で除去することがで
き、本発明は高品位アルミニウム材に対する要請
に応える優れた工業的発明である。[Table] Effects of the invention According to the present invention, for filtration of molten aluminum,
By performing pressure filtration using a filter with a fine pore size, which has not been attempted before, fine inclusions in aluminum can be removed with high removal efficiency, and the present invention is an excellent product that meets the demand for high-grade aluminum materials. It is an industrial invention.
第１図はアルミニウム溶湯の濾過における瀘材
の平均気孔径と介在物除去効果の関係を示す図面
で、第２図は本発明に使用した濾過装置の概略構
造を示す縦断面図である。
１……装置本体、２……るつぼ、３……電熱コ
イル、４……加圧蓋、５……不活性ガス導管、６
……フイルター、７……樋。
FIG. 1 is a drawing showing the relationship between the average pore diameter of the filter material and the inclusion removal effect in filtration of molten aluminum, and FIG. 2 is a longitudinal sectional view showing the schematic structure of the filtration device used in the present invention. 1... Apparatus body, 2... Crucible, 3... Electric heating coil, 4... Pressurizing lid, 5... Inert gas conduit, 6
...Filter, 7...Gutter.
Claims (1)
する方法において、平均気孔径が10〜50μｍであ
るフイルターを使用し、フイルター部での濾過速
度が0.05〜0.8cm／secとなるように加圧濾過する
ことを特徴とするアルミニウム溶湯の濾過方法。 ２ 前記フイルターが、Al2O3、SiCまたはSi3N4
を主成分とするセラミツク材を骨材とするもので
ある特許請求の範囲第１項記載のアルミニウム溶
湯の濾過方法。[Claims] 1. In a method of filtering aluminum or aluminum alloy, a filter having an average pore diameter of 10 to 50 μm is used, and pressure is applied so that the filtration rate at the filter part is 0.05 to 0.8 cm/sec. A filtration method for molten aluminum characterized by filtration. 2 The filter is Al 2 O 3 , SiC or Si 3 N 4
2. The method for filtering molten aluminum according to claim 1, wherein the aggregate is a ceramic material containing as a main component.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62047807A JPS63216933A (en) | 1987-03-04 | 1987-03-04 | Filtration method for molten aluminum |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62047807A JPS63216933A (en) | 1987-03-04 | 1987-03-04 | Filtration method for molten aluminum |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63216933A JPS63216933A (en) | 1988-09-09 |
| JPH0422977B2 true JPH0422977B2 (en) | 1992-04-21 |
Family
ID=12785636
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62047807A Granted JPS63216933A (en) | 1987-03-04 | 1987-03-04 | Filtration method for molten aluminum |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63216933A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH03281738A (en) * | 1990-03-30 | 1991-12-12 | Ngk Insulators Ltd | Filter material for metallic molten metal and method for filtering metallic molten metal by using the same |
| JP5368663B2 (en) * | 2000-04-14 | 2013-12-18 | トーソー エスエムディー，インク． | Sputter target for reducing particulate emission during spattering and method for manufacturing the same |
| MY138532A (en) | 2000-08-31 | 2009-06-30 | Foseco Int | Refractory articles |
-
1987
- 1987-03-04 JP JP62047807A patent/JPS63216933A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63216933A (en) | 1988-09-09 |
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