WO2014091939A1 - ケイ素含有アルミニウム合金鋳塊の製造方法 - Google Patents
ケイ素含有アルミニウム合金鋳塊の製造方法 Download PDFInfo
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- WO2014091939A1 WO2014091939A1 PCT/JP2013/082093 JP2013082093W WO2014091939A1 WO 2014091939 A1 WO2014091939 A1 WO 2014091939A1 JP 2013082093 W JP2013082093 W JP 2013082093W WO 2014091939 A1 WO2014091939 A1 WO 2014091939A1
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- silicon
- aluminum alloy
- ingot
- containing aluminum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D1/00—Treatment of fused masses in the ladle or the supply runners before casting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C21/00—Alloys based on aluminium
- C22C21/02—Alloys based on aluminium with silicon as the next major constituent
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D21/00—Casting non-ferrous metals or metallic compounds so far as their metallurgical properties are of importance for the casting procedure; Selection of compositions therefor
- B22D21/02—Casting exceedingly oxidisable non-ferrous metals, e.g. in inert atmosphere
- B22D21/04—Casting aluminium or magnesium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/026—Alloys based on aluminium
Definitions
- the present invention relates to a production method for producing a silicon-containing aluminum alloy ingot containing a small amount of impurity phosphorus.
- the silicon lump used as a raw material for producing a continuous casting rod of a silicon-containing aluminum alloy contains phosphorus. It is considered that such impurity phosphorus in the silicon lump is brought from the raw material meteorite and carbon used for reduction in the process of producing the silicon lump.
- Patent Document 1 describes that phosphorus is removed by filtering an aluminum alloy melt containing 5 ppm or more of phosphorus at a melt temperature of 750 ° C. or less.
- Patent Document 2 oxygen is added together with MgO in Al or Al alloy molten metal containing P as an impurity to form an oxide of impurity P and / or a composite oxide of P and Mg. It is described that the impurity phosphorus is removed by separation.
- Patent Document 3 Mg is added to a molten aluminum containing P at a molten metal temperature of 650 to 850 ° C. to form a compound of P and Mg, and chlorine gas or chloride is blown to form MgCl 2. It is described that MgCl 2 is allowed to float while absorbing a compound of P and Mg to remove P in the molten metal.
- Ca is added to a molten aluminum containing P at a molten metal temperature of 650 to 850 ° C. to form a compound of P and Ca, and chlorine gas or chloride is blown to form CaCl 2. Further, it is also described that the CaCl 2 is floated while absorbing a compound of P and Mg to remove P in the molten metal.
- JP-A-4-276031 Japanese Patent Laid-Open No. 7-207366 Japanese Patent No. 3524519
- Patent Documents 1 to 3 have the following problems. That is, in the technique of Patent Document 1, since fine aluminum phosphide particles are also mixed, there is a problem that there is phosphorus that cannot be removed by passing through the filtration filter. There was a problem of causing clogging.
- Patent Document 2 has a problem in that oxygen is blown into the molten metal, resulting in an oxidation loss (aluminum loss) of the molten metal.
- the present invention has been made in view of such a technical background, and can prevent clogging of a filter such that casting must be stopped, suppress aluminum loss, and obtain silicon-containing aluminum obtained.
- An object of the present invention is to provide a method for producing a silicon-containing aluminum alloy ingot that can sufficiently reduce the content of impurity phosphorus in the alloy ingot.
- phosphorus is present as a phosphorus compound or the like in the stage of reducing the meteorite with carbon to form an ingot, but this impurity phosphorus is present in the final solidification part of the silicon ingot, etc.
- the present inventor found out that the surface of the final solidified portion is distributed at a high concentration, and as a result of intensive research based on such new knowledge, the water washing treatment before putting the silicon lump into the melting furnace
- the inventors have found that the phosphorus content of impurities in the resulting silicon-containing aluminum alloy ingot can be reduced, and the present invention has been completed. That is, in order to achieve the above object, the present invention provides the following means.
- a water washing step of performing a water washing treatment on a silicon lump containing phosphorus as an impurity A molten metal forming step for obtaining a molten metal by charging an aluminum raw material and an alloy raw material containing at least a silicon block obtained through the water washing step into a melting furnace; And a casting step of obtaining a silicon-containing aluminum alloy ingot by casting the obtained molten metal, and a method for producing a silicon-containing aluminum alloy ingot.
- the silicon ingot is crushed to obtain a plurality of crushed materials,
- a silicon ingot containing phosphorus as an impurity is crushed to obtain a plurality of crushed materials, and then a water washing treatment for washing the surface of the crushed material with water is performed.
- a water washing treatment for washing the surface of the crushed material with water is performed.
- a molten metal forming step in which an alloy raw material including at least an aluminum raw material and a washed silicon lump is charged into a melting furnace to obtain a molten metal; And a casting step of obtaining a silicon-containing aluminum alloy ingot by casting the obtained molten metal, and a method for producing a silicon-containing aluminum alloy ingot.
- the silicon lump that has been subjected to the water washing treatment before being put into the melting furnace is used as at least a part of the silicon lump as a raw material used for producing the silicon-containing aluminum alloy ingot, Phosphorus (including phosphorus compounds) that is often agglomerated on the surface of the lump can be sufficiently washed away, and a silicon-containing aluminum alloy ingot with a sufficiently reduced content of impurity phosphorus can be produced. It becomes possible to suppress the phosphorus content in the silicon-containing aluminum alloy ingot to 5 ppm or less.
- the filter can be prevented from being clogged so that casting must be stopped, so that productivity can be further improved.
- the water-washing treatment is performed in the state of the pulverized product obtained by pulverization, so that it is possible to produce a silicon-containing aluminum alloy ingot with a further reduced content of impurity phosphorus.
- the temperature of water used for the water washing treatment is 5 ° C. to 90 ° C., so that it is possible to further improve the dissolution and removal of phosphorus by water washing.
- the silicon lump that has already been washed with water is used as at least a part of the silicon lump used as a raw material for the production of the silicon-containing aluminum alloy ingot, the phosphorus content of impurities is sufficiently high. Reduced silicon-containing aluminum alloy ingots can be produced. It becomes possible to suppress the phosphorus content in the silicon-containing aluminum alloy ingot to 5 ppm or less. Moreover, the aluminum loss can be sufficiently suppressed, and the filter can be prevented from being clogged so that the casting must be stopped, thereby improving the productivity.
- the manufacturing method of the present invention includes a water washing step, a molten metal forming step, and a casting step.
- a silicon lump (silicon lump containing phosphorus as an impurity) used as a raw material is washed with water.
- phosphorus is present as a phosphorus compound or the like in the stage of reducing the meteorite with carbon to form an ingot, but as described above, this impurity phosphorus is the final solidification of the silicon ingot.
- the present inventor has found that a high concentration is distributed on the surface, particularly on the surface of the final solidified portion.
- the final solidified portion is that when molten silicon is poured into the mold 10, the molten silicon is cooled and solidified from the vicinity of the wall surface of the mold, and finally the molten silicon on the opening surface of the upper part of the mold 10.
- the upper surface portion solidifies last, which means the solidified portion that solidifies last. For example, after 95% or more of the volume of molten silicon in the mold is solidified, a portion where the remaining molten silicon is finally solidified can be defined as a “final solidified portion” (upper solidified portion).
- the water washing step for example, at least the surface of the final solidified part (the upper surface of the ingot 11) of the silicon ingot 11 is washed with water 13 (see FIG. 1). After drying the washed silicon ingot 11, the silicon ingot 11 is crushed (crushed) to obtain a plurality of crushed materials 12, and these crushed materials 12 are put into a melting furnace in the next step.
- the silicon ingot 11 is crushed to obtain a plurality of crushed materials 12, and a water washing process is performed in which the surfaces of the crushed materials 12 are washed with water 13 (see FIGS. 2 and 3). After the adhering water of the silicon crushed material 12 that has undergone the cleaning is removed by drying, wiping, or the like, the plurality of crushed materials 12 are put into a melting furnace in the next step.
- the size of the crushed material is preferably 30 cm or less (including powder form) as an average value of the major axis.
- the size of the crushed material is preferably in the range of 1 cm to 30 cm in terms of the average value of the major axis.
- the powdery powder produced during crushing may be put into the melting furnace together with the crushed material of 1 to 30 cm in the subsequent molten metal forming step.
- the water washing treatment may be performed by spraying water 13 on a silicon ingot, crushed material, or the like (see FIGS. 1 and 2), or may be performed by immersing the silicon ingot, crushed material, or the like in water 13 (FIG. 1). 3), and the method is not particularly limited.
- the silicon ingot When the silicon ingot is sprayed with water and washed with water, it is preferable that the silicon ingot is sprayed with water from the upper side with the final solidified portion facing upward. Moreover, when spraying water to a crushed material and performing a water-washing process, it is preferable to perform the spray from a horizontal direction (horizontal direction) in addition to the spray from an upper side.
- ⁇ ⁇ When performing the water washing treatment, it is preferable to wash with 100 to 1000 parts by mass of water (water for immersion or spray water) per 100 parts by mass of the silicon ingot or crushed material.
- the washing time is preferably set to 10 to 30 minutes.
- the temperature of water during the washing treatment is 5 ° C to 90 ° C.
- the temperature of water is more preferably 40 ° C. to 60 ° C. in the case where the silicon lump is transported and moved in a later step. By setting the temperature to 40 ° C. to 60 ° C., work safety can be improved.
- phosphorus including a phosphorus compound
- a silicon lump such as a silicon ingot
- molten metal forming step an aluminum raw material and an alloy raw material containing at least a silicon lump obtained through the water washing step are charged into a melting furnace and melted to obtain a molten metal.
- the molten metal temperature for melting is usually in the range of 770 ° C. to 870 ° C.
- the aluminum material is not particularly limited, and examples thereof include aluminum ingots.
- Examples of the “silicon lump obtained through the water washing step” include silicon ingots that have undergone the water washing step, silicon crushed materials that have undergone the water washing step, and the like.
- the silicon lump that has not been subjected to the water washing treatment together with the above-mentioned “silicon lump obtained through the water washing step” depends on the intended alloy specifications. Needless to say, it is desirable that the silicon lump that has not been subjected to such a water washing treatment should not be added as much as possible in the alloy specification for the purpose of sufficiently obtaining the impurity phosphorus content reduction effect.
- the molten metal obtained in the molten metal forming step is cast to obtain an aluminum alloy ingot (silicon-containing aluminum alloy ingot) containing silicon.
- the casting may be processed into a silicon-containing aluminum alloy ingot or may be processed into a silicon-containing aluminum alloy continuous casting rod, and the shape of the ingot obtained by casting is not particularly limited.
- the casting method is not particularly limited, and examples thereof include a semi-continuous casting method, a horizontal continuous casting method, a strip casting method, and a gravity casting method, but any casting method can be used.
- the production method of the present invention is for producing a silicon-containing aluminum alloy ingot (silicon-containing aluminum alloy cast product), and there are no particular restrictions on other components other than Al and Si. It is preferable to use 2000 series alloy, 3000 series alloy, 4000 series alloy, 5000 series alloy, and 6000 series alloy. In particular, the effect (effect of the present invention) when an alloy system containing a large amount of Si, for example, a 4000 series alloy is large is preferable.
- Example 1 A silicon ingot 11 having a rectangular parallelepiped shape was obtained by heating and melting a silicon lump (phosphorus content 230 ppm) obtained by reducing the meteorite and casting it into a mold 10 for natural cooling. By this natural cooling, solidification of the molten silicon progressed from the vicinity of the outer peripheral frame portion of the mold, and the solidification was completed on the upper exposed surface. As shown in FIG. 1, with the silicon ingot 11 held in the mold 10, a water washing treatment was performed by spraying water 13 at 20 ° C. for 30 minutes on the upper surface (final solidified portion) of the ingot 11.
- a rectangular parallelepiped silicon ingot 11 is taken out from the mold 10 and the adhering water is removed by drying. Then, the silicon ingot is crushed to obtain a large number of crushed materials 12, and these crushed materials 12 are put into a melting furnace. Furthermore, an aluminum ingot with an aluminum content of 99.7% by mass, a copper ingot with a copper content of 99.9% by mass, and a magnesium ingot with a magnesium content of 99.9% by mass are charged into the melting furnace.
- the aluminum alloy melt was prepared by heating to 850 ° C. Each material was charged so that the silicon content in the molten aluminum alloy was 11 mass%, the copper content was 4 mass%, the magnesium content was 0.5 mass%, and the aluminum content was 84.5 mass%. .
- the average value of the major axis is 10 cm.
- a silicon-containing aluminum alloy ingot (silicon-containing aluminum alloy ingot) was obtained by casting the molten aluminum alloy.
- Example 2 A silicon block obtained by reducing the meteorite (phosphorus content is the same as the phosphorus content of the silicon block used in Example 1) is heated and melted and poured into the mold 10 to be naturally cooled to form a rectangular parallelepiped shape. The silicon ingot 11 was obtained. By this natural cooling, solidification of the molten silicon progressed from the vicinity of the outer peripheral frame portion of the mold, and the solidification was completed on the upper exposed surface.
- a rectangular parallelepiped silicon ingot 11 was taken out from the mold 10, and the silicon ingot was crushed to obtain a large number of crushed objects 12. Thereafter, a water washing treatment was performed in which the crushed material 12 was immersed in water 13 at 90 ° C. for 10 minutes. Next, after removing the adhering water from the crushed material 12 taken out by drying, the crushed material 12 is put into a melting furnace, and the aluminum content is 99.7% by mass, and the copper content is 99.9%. A mass of copper ingot and magnesium ingot having a magnesium content of 99.9 mass% were put into a melting furnace and heated to 850 ° C. to prepare a molten aluminum alloy.
- each material was charged so that the silicon content in the molten aluminum alloy was 11 mass%, the copper content was 4 mass%, the magnesium content was 0.5 mass%, and the aluminum content was 84.5 mass%. .
- the average value of the major axis is 15 cm.
- a silicon-containing aluminum alloy ingot (silicon-containing aluminum alloy ingot) was obtained by casting the molten aluminum alloy.
- a rectangular parallelepiped silicon ingot is taken out from the mold, and a large number of pulverized products obtained by pulverizing the silicon ingot are put into a melting furnace. Further, an aluminum ingot having an aluminum content of 99.7% by mass, copper A copper ingot with a content of 99.9% by mass and a magnesium ingot with a magnesium content of 99.9% by mass were put into a melting furnace and heated to 850 ° C. to prepare a molten aluminum alloy. Each material was charged so that the silicon content in the molten aluminum alloy was 11 mass%, the copper content was 4 mass%, the magnesium content was 0.5 mass%, and the aluminum content was 84.5 mass%. . As for the size of the crushed material, the average value of the major axis is 10 cm.
- a silicon-containing aluminum alloy ingot (silicon-containing aluminum alloy ingot) was obtained by casting the molten aluminum alloy.
- the silicon-containing aluminum alloy ingots of Examples 1 and 2 produced by the production method of the present invention had a sufficiently low phosphorus content.
- the silicon-containing aluminum alloy ingot of Comparative Example 1 manufactured without using the manufacturing method of the present invention had a phosphorus content of 25 ppm and a high phosphorus content.
- the silicon-containing aluminum alloy ingot manufactured by the manufacturing method of the present invention has a low content of impurity phosphorus, for example, 1) Products and parts (specifically, for example, automobile casting parts, etc.) that have a high impurity phosphorus content that may cause cracks at the aggregate of phosphorus when external stress is applied. 2) Products and parts (specifically, for example, foils for electrolytic capacitors) obtained by processing (rolling, extruding, forging, etc.) by applying materials and external stresses that are manufactured through processes involving chemical reactions such as chemical etching. , Plate materials, auto parts, etc.) However, it is not particularly limited to these exemplified uses.
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Abstract
Description
アルミニウム原料及び前記水洗工程を経て得られたケイ素塊を少なくとも含む合金原料を溶解炉に投入して溶融させて溶湯を得る溶湯形成工程と、
前記得られた溶湯を鋳造加工することによって、ケイ素を含有するアルミニウム合金の鋳塊を得る鋳造工程と、を含むことを特徴とするケイ素含有アルミニウム合金鋳塊の製造方法。
前記解砕物を、前記溶湯形成工程で溶解炉に投入する前項1に記載のケイ素含有アルミニウム合金鋳塊の製造方法。
前記水洗処理後の解砕物を、前記溶湯形成工程で溶解炉に投入する前項1に記載のケイ素含有アルミニウム合金鋳塊の製造方法。
前記得られた溶湯を鋳造加工することによって、ケイ素を含有するアルミニウム合金の鋳塊を得る鋳造工程と、を含むことを特徴とするケイ素含有アルミニウム合金鋳塊の製造方法。
硅石を還元処理することにより得られたケイ素塊(リン含有率230ppm)を加熱溶融させたものを鋳型10に流し込んで自然冷却させて直方体形状のケイ素インゴット11を得た。この自然冷却により、溶融ケイ素の凝固は、鋳型外周枠部の近傍から進行し上側露出面で凝固が完了した。図1に示すようにケイ素インゴット11を鋳型10内に留めた状態で該インゴット11の上面(最終凝固部)に20℃の水13を30分間噴霧する水洗処理を行った。
硅石を還元処理することにより得られたケイ素塊(リン含有率は実施例1で用いたケイ素塊のリン含有率と同一)を加熱溶融させたものを鋳型10に流し込んで自然冷却させて直方体形状のケイ素インゴット11を得た。この自然冷却により、溶融ケイ素の凝固は、鋳型外周枠部の近傍から進行し上側露出面で凝固が完了した。
硅石を還元処理することにより得られたケイ素塊(リン含有率は実施例1で用いたケイ素塊のリン含有率と同一)を加熱溶融させたものを鋳型に流し込んで自然冷却させた。この自然冷却により、溶融ケイ素の凝固は、鋳型外周枠部の近傍から進行し上側露出面で凝固が完了した。
ケイ素含有アルミニウム合金鋳塊におけるリンの定量分析は、発光分析装置(島津製作所製「PDA 5500II」)を用いて行った。
1)不純物のリンの含有率が高いものであると外部応力が加わった際にリンの凝集部が割れの起点になる恐れのある製品、部品(具体的には、例えば、自動車鋳物部品など)
2)化学エッチング等の化学反応を伴う工程を経て製造される素材及び外部応力を加えて加工して(圧延、押出、鍛造等)得る製品、部品(具体的には、例えば、電解コンデンサー用箔、板素材、自動車部品など)
として好適に用いられるが、特にこれら例示の用途に限定されるものではない。
12…解砕物(ケイ素塊)
13…水
Claims (6)
- 不純物としてリンを含有したケイ素塊に水洗処理を行う水洗工程と、
アルミニウム原料及び前記水洗工程を経て得られたケイ素塊を少なくとも含む合金原料を溶解炉に投入して溶融させて溶湯を得る溶湯形成工程と、
前記得られた溶湯を鋳造加工することによって、ケイ素を含有するアルミニウム合金の鋳塊を得る鋳造工程と、を含むことを特徴とするケイ素含有アルミニウム合金鋳塊の製造方法。 - 前記水洗工程において、不純物としてリンを含有したケイ素インゴットの表面を水で洗浄する水洗処理を行った後、該ケイ素インゴットを解砕して複数個の解砕物を得、
前記解砕物を、前記溶湯形成工程で溶解炉に投入する請求項1に記載のケイ素含有アルミニウム合金鋳塊の製造方法。 - 前記水洗工程において、不純物としてリンを含有したケイ素インゴットを解砕して複数個の解砕物を得た後、前記解砕物の表面を水で洗浄する水洗処理を行い、
前記水洗処理後の解砕物を、前記溶湯形成工程で溶解炉に投入する請求項1に記載のケイ素含有アルミニウム合金鋳塊の製造方法。 - 前記水洗処理に用いる水の温度が5℃~90℃である請求項1~3のいずれか1項に記載のケイ素含有アルミニウム合金鋳塊の製造方法。
- アルミニウム原料及び水洗されたケイ素塊を少なくとも含む合金原料を溶解炉に投入して溶融させて溶湯を得る溶湯形成工程と、
前記得られた溶湯を鋳造加工することによって、ケイ素を含有するアルミニウム合金の鋳塊を得る鋳造工程と、を含むことを特徴とするケイ素含有アルミニウム合金鋳塊の製造方法。 - 前記鋳造加工で得られたケイ素含有アルミニウム合金鋳塊におけるリン含有率が5ppm以下である請求項1~5のいずれか1項に記載のケイ素含有アルミニウム合金鋳塊の製造方法。
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EP13863450.6A EP2929958A4 (en) | 2012-12-10 | 2013-11-28 | PROCESS FOR PRODUCING ALUMINUM ALLOY INGOT CONTAINING SILICON |
US14/443,666 US20150314367A1 (en) | 2012-12-10 | 2013-11-28 | Method of producing silicon-containing aluminum alloy ingot |
JP2014551971A JP5833257B2 (ja) | 2012-12-10 | 2013-11-28 | ケイ素含有アルミニウム合金鋳塊の製造方法 |
CN201380064224.2A CN104837577B (zh) | 2012-12-10 | 2013-11-28 | 含硅的铝合金铸块的制造方法 |
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FR2814757B1 (fr) * | 2000-10-02 | 2003-07-11 | Invensil | Elaboration d'alliages de type aluminium-silicium |
WO2010126639A1 (en) * | 2009-04-29 | 2010-11-04 | Calisolar, Inc. | Process control for umg-si material purification |
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2013
- 2013-11-28 US US14/443,666 patent/US20150314367A1/en not_active Abandoned
- 2013-11-28 KR KR1020157011677A patent/KR20150067291A/ko not_active Application Discontinuation
- 2013-11-28 CN CN201380064224.2A patent/CN104837577B/zh not_active Expired - Fee Related
- 2013-11-28 JP JP2014551971A patent/JP5833257B2/ja not_active Expired - Fee Related
- 2013-11-28 WO PCT/JP2013/082093 patent/WO2014091939A1/ja active Application Filing
- 2013-11-28 EP EP13863450.6A patent/EP2929958A4/en not_active Withdrawn
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113355543A (zh) * | 2021-05-27 | 2021-09-07 | 江苏奋杰有色金属制品有限公司 | 一种铝合金铸棒的生产工艺 |
Also Published As
Publication number | Publication date |
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CN104837577A (zh) | 2015-08-12 |
US20150314367A1 (en) | 2015-11-05 |
CN104837577B (zh) | 2016-08-24 |
KR20150067291A (ko) | 2015-06-17 |
EP2929958A1 (en) | 2015-10-14 |
JP5833257B2 (ja) | 2015-12-16 |
EP2929958A4 (en) | 2016-07-13 |
JPWO2014091939A1 (ja) | 2017-01-05 |
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