JP3903829B2 - Mg alloy recycling method, recycling agent, and manufacturing method of recycling agent - Google Patents
Mg alloy recycling method, recycling agent, and manufacturing method of recycling agent Download PDFInfo
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Description
【０００１】
【発明の属する技術分野】
本発明は、Ｍｇ合金をリサイクルする方法、リサイクル剤およびリサイクル剤の製造方法に関する。
【０００２】
【従来の技術】
資源の有効活用とコスト低減の観点から、Ｍｇ合金スクラップを溶解・鋳造用の原料として再利用すなわちリサイクルすることが行なわれている。このようにしてＭｇ合金をリサイクルする際には、下記の２点Ｑ１、Ｑ２が重要である。
【０００３】
（Ｑ１）Ｍｇ合金スクラップ中のＦｅ分を除去する必要がある。Ｆｅが残存するとＭｇ合金の耐食性が低下する。
【０００４】
（Ｑ２）鋳造組織を微細化する処理が必要である。Ｍｇ合金スクラップを単に溶解して鋳造すると、鋳造組織が粗粒化して強度の低下を招く。
【０００５】
そのため、従来は下記の手段Ａ１、Ａ２が採られていた。（例えば、「マグネシウム技術便覧」日本マグネシウム協会編（発行日：２０００年５月１７日）を参照。）
（Ａ１）Ｆｅ分を除去するために、Ｍｇ合金溶湯中にＡｌ−１０％Ｍｎ合金を投入して、金属間化合物（ＦｅＭｎ）Ａｌ６を生成させ、その沈殿分離によりＦｅを溶湯中から除去する。
【０００６】
（Ａ２）鋳造組織を微細化するために、Ｍｇ合金溶湯中に微細化剤としてヘキサクロロエタン（Ｃ２Ｃｌ６）を添加する。
【０００７】
しかし上記従来の方法には、下記の問題があった。
【０００８】
まず、要件Ｑ１、Ｑ２を共に満たすためには手段Ａ１、Ａ２を両方実施する必要がある。すなわち、Ａｌ−１０％Ｍｎ合金（Ａ１）には微細化効果（Ｑ２）はなく、ヘキサクロロエタン（Ａ２）にはＦｅ分除去効果（Ｑ１）はない。
【０００９】
また、ヘキサクロロエタンは、有害な塩素化炭化水素（ＣＨＣ）を発生するため、環境保護の観点から望ましくない。
【００１０】
【発明が解決しようとする課題】
本発明は、上記従来技術の問題を解消し、環境に有害な添加剤を用いることなく、Ｆｅ分の除去と鋳造組織の微細化とを同時に達成できるＭｇ合金のリサイクル方法、リサイクル剤、リサイクル剤の製造方法を提供することを目的とする。
【００１１】
【課題を解決するための手段】
上記の目的を達成するために、本発明のＭｇ合金のリサイクル方法は、下記の工程：
Ｍｇ粉末とＭｎＢ粉末とＡｌ粉末との混合粉末を加圧成形する工程、
得られた成形体を熱処理することにより該成形体内にＡｌＢ２を内部生成させる工程、および
得られたＡｌＢ２含有成形体をＭｇ合金溶湯に添加する工程
を含むことを特徴とする。
【００１２】
また、本発明のＭｇ合金のリサイクル剤は、Ｍｇ粒子、Ｍｎ粒子、Ａｌ粒子および少なくともＡｌＢ２粒子を含むＡｌ−Ｂ化合物粒子が混在する成形体から成ることを特徴とする。
【００１３】
更に、本発明のＭｇ合金のリサイクル剤の製造方法は、下記の工程：
Ｍｇ粉末とＭｎＢ粉末とＡｌ粉末との混合粉末を加圧成形する工程、および
得られた成形体を熱処理することにより該成形体内にＡｌＢ２を内部生成させる工程
を含むことを特徴とする。
【００１４】
【発明の実施の形態】
本発明のＭｇ合金のリサイクル方法においては、Ｍｇ粉末とＭｎＢ粉末とＡｌ粉末との混合粉末を加圧成形し、得られた成形体を熱処理することにより該成形体内にＡｌＢ２を内部生成させる。ＡｌＢ２の内部生成は典型的には下記の反応により行なわれる。
【００１５】
２ＭｎＢ＋Ａｌ→２Ｍｎ＋ＡｌＢ２……(A)
熱処理された成形体は、Ｍｇ粒子、Ｍｎ粒子およびＡｌ粒子から成る金属マトリクス中にＡｌＢ２金属間化合物粒子が分散した粒子分散型金属基複合材料の状態になっていると言える。
【００１６】
次に、上記で得られたＡｌＢ２含有成形体をＭｇ合金溶湯に添加すると、Ｍｇ粒子、Ｍｎ粒子およびＡｌ粒子から成る金属マトリクスは溶湯中に溶解して、溶湯と下記のように反応する。
【００１７】
Ｍｎ＋６Ａｌ＋Ｆｅ→（ＦｅＭｎ）Ａｌ６……(B)
これにより、Ｍｇ合金中のＦｅは金属間化合物（ＦｅＭｎ）Ａｌ６として固定され、沈殿分離により溶湯から除去される。
【００１８】
同時に、溶湯中への金属マトリクスの溶解に伴い、ＡｌＢ２粒子が溶湯中に分散する。内部生成ＡｌＢ２粒子はサブミクロン〜１μｍ程度の微細な粒子であり、多数の微細な凝固核として作用し、微細な鋳造組織を生成させる。
【００１９】
このように本発明によれば、Ｍｇ合金中のＦｅ分の除去と鋳造組織の微細化とを同時に行なうことができる。
【００２０】
しかも、本発明においては、従来のようにヘキサクロロエタンのような環境に有害な添加剤を用いることがないので、環境保護の観点からも問題を生じない。
【００２１】
なお、成形体の構成成分であるＭｇは、上記反応(A)(B)のいずれにも関与していない。しかし、熱処理後の成形体をＭｇ溶湯に添加した際に、成形体の濡れ性を確保し、溶湯中への金属マトリクスの溶解とＡｌＢ２粒子の分散とを実現するためにＭｇは不可欠な構成成分である。
【００２２】
成形体を構成するＭｎＢ粉末とＡｌ粉末の配合比は、前記反応(A)に対応するＡｌとＢとの化学量論比（原子比でＡｌ：Ｂ＝１：２）と、前記反応(B)に対応するＭｎとＡｌとの化学量論比（原子比でＭｎ：Ａｌ＝１：６）とを共に満たすように設定することを標準とする。Ｍｇ粉末の配合比は、成形体とＭｇ合金溶湯との濡れ性を確保するのに十分な量に設定できる。これらの条件をまとめると、反応式(A)(B)を下記(A')(B'）のように表現することができる。
【００２３】
αＭｇ＋２ＭｎＢ＋１３Ａｌ→αＭｇ＋２Ｍｎ＋１２Ａｌ＋ＡｌＢ２…(A')
２Ｍｎ＋１２Ａｌ＋２Ｆｅ→２（ＦｅＭｎ）Ａｌ６……(B')
ここで、各係数は成形体原料粉末の配合比に対応しており、Ｍｇの係数αは一般に数１０以上の大きい数値（配合比）になる。
【００２４】
【実施例】
下記の条件および手順によりＭｇ合金のリサイクル処理を行なった。
【００２５】
まず、Ｍｇ粉末、ＭｎＢ粉末およびＡｌ粉末を表１に示した配合比になるように秤量し、Ｖ型混粉機にて３０分混合した。
【００２６】
【表１】
得られた混合粉末を、成形圧７ton/cm２で加圧成形し、円柱状成形体（φ３０mm、２０ｇ／個）を作製した。
【００２８】
この成形体をＡｒ雰囲気中にて表２に示した各温度でそれぞれ１時間熱処理した。
【００２９】
【表２】
表３に示す組成のＭｇ合金スクラップを溶解してＭｇ合金溶湯を形成した。
【００３１】
【表３】
上記Ｍｇ合金溶湯２０００ｇを７５０℃に保持し、上記各熱処理後の成形体を表２に示した添加量で添加した。
【００３３】
成形体を添加した溶湯を下記の条件にて鋳造した。
【００３４】
〔鋳造条件〕
鋳造方法 ：重力鋳造
鋳型 ：ＪＩＳ４号試験片用舟金型
鋳型予熱温度 ：１００℃
添加時溶湯温度：７５０℃
鋳造時溶湯温度：７５０℃
得られた各鋳造品について、Ｆｅ含有量の分析および結晶粒径の測定を行なった結果を表２に示す。
【００３５】
Ｆｅ含有量は、原料スクラップの０.０１４mass％に対して、成形体の熱処理を８００℃で行なった実験No.１〜３では０.０１４mass％であり、原料スクラップと同等であったが、成形体の熱処理を１０００℃または１２００℃で行なった実験No.４〜９では０.００４mass％であり顕著に低減した。いずれの場合も、添加量の影響は認められなかった。なお、成形体無添加の場合は原料スクラップと同等であることを確認した。図１に、添加によるＦｅ除去効果が得られた実験No.４〜９と無添加の実験No.１０について、鋳造品のＦｅ含有量を対比して示す。
【００３６】
結晶粒径は、成形体無添加の場合の３００μｍに対して、成形体の熱処理を８００℃で行なった実験No.１〜３では３００μｍであり、無添加の実験No.１０と同等であったが、成形体の熱処理を１０００℃または１２００℃で行なった実験No.４〜９では５０〜２００μｍであり明瞭な細粒化効果が認められた。更に、熱処理温度１０００℃の実験No.４〜６の方が、熱処理温度１２００℃の実験No.７〜９よりも微細化効果が大きかった。
【００３７】
上記の結果は下記のように解釈できる。
【００３８】
８００℃では、前記反応(A)(B)はどちらも起きないため、反応(A)の生成物ＡｌＢ２による細粒化効果も、反応(B)によるＦｅ除去効果も得られない。
【００３９】
１０００℃および１２００℃では、反応(A)(B)のどちらも起きるため、反応(A)の生成物ＡｌＢ２による細粒化効果および反応(B)によるＦｅ除去効果の両方が得られる。また、１０００℃に対して細粒化効果が小さい１２００℃では、反応(A)によるＡｌＢ２の生成に加えて下記反応(C)によってＡｌＢ１２の生成も起きており、その分だけＡｌＢ２の生成量が少ない。１２００℃の熱処理で生成するＡｌＢ１２は凝固核として機能しないため細粒化には寄与せず、細粒化作用を持つＡｌＢ２の生成量が減少した分だけ細粒化効果が小さくなる。
【００４０】
αＭｇ＋１２ＭｎＢ＋１３Ａｌ→αＭｇ＋１２Ｍｎ＋１２Ａｌ＋ＡｌＢ１２………(C)
なお、Ａｌ−Ｂ２元系では６６０℃以上でＡｌＢ２が生成し、９７５℃以上でＡｌＢ１２が生成するが、多量のＭｇの存在が前提となる多元系としてのＭｇ合金中では、上記各生成温度が高温側にシフトしたと考えられる。
【００４１】
【発明の効果】
以上説明したように、本発明によれば、環境に有害な添加剤を用いることなく、Ｆｅ分の除去と鋳造組織の微細化とを同時に達成できるＭｇ合金のリサイクル方法、リサイクル剤、リサイクル剤の製造方法が提供される。
【図面の簡単な説明】
【図１】図１は、本発明によるリサイクル処理を行なった場合と無処理の場合とについてＦｅ含有量を比較して示すグラフである。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method of recycling an Mg alloy, a recycling agent, and a manufacturing method of the recycling agent.
[0002]
[Prior art]
From the viewpoint of effective use of resources and cost reduction, Mg alloy scrap is reused, that is, recycled as a raw material for melting and casting. When recycling the Mg alloy in this way, the following two points Q1 and Q2 are important.
[0003]
(Q1) It is necessary to remove the Fe content in the Mg alloy scrap. If Fe remains, the corrosion resistance of the Mg alloy decreases.
[0004]
(Q2) A process for refining the cast structure is necessary. If the Mg alloy scrap is simply melted and cast, the cast structure becomes coarse and the strength decreases.
[0005]
Therefore, conventionally, the following means A1 and A2 have been adopted. (For example, see “Magnesium Technical Handbook” edited by Japan Magnesium Association (issue date: May 17, 2000).)
(A1) In order to remove the Fe content, an Al-10% Mn alloy is introduced into the molten Mg alloy to form an intermetallic compound (FeMn) Al 6, and Fe is removed from the molten metal by precipitation separation. .
[0006]
(A2) In order to refine the cast structure, hexachloroethane (C 2 Cl 6 ) is added as a refiner in the molten Mg alloy.
[0007]
However, the conventional method has the following problems.
[0008]
First, in order to satisfy both requirements Q1 and Q2, it is necessary to implement both means A1 and A2. That is, the Al-10% Mn alloy (A1) does not have a refinement effect (Q2), and the hexachloroethane (A2) does not have an Fe content removal effect (Q1).
[0009]
Further, hexachloroethane is undesirable from the viewpoint of environmental protection because it generates harmful chlorinated hydrocarbons (CHC).
[0010]
[Problems to be solved by the invention]
The present invention solves the above-described problems of the prior art, and can simultaneously remove the Fe content and refine the cast structure without using an additive harmful to the environment, a recycling method of Mg alloy, a recycling agent, and a recycling agent. It aims at providing the manufacturing method of.
[0011]
[Means for Solving the Problems]
In order to achieve the above object, the Mg alloy recycling method of the present invention comprises the following steps:
A step of pressure-molding a mixed powder of Mg powder, MnB powder and Al powder,
Step of internally generate AlB 2 in the molding body by heat treating the obtained molded body, and the resulting AlB 2 containing shaped body, characterized in that it comprises the step of adding the Mg alloy melt.
[0012]
The Mg alloy recycle agent of the present invention is characterized by comprising a molded body in which Mg particles, Mn particles, Al particles and Al—B compound particles containing at least AlB 2 particles are mixed.
[0013]
Furthermore, the manufacturing method of the recycling agent of Mg alloy of this invention is the following process:
It includes a step of pressure-molding a mixed powder of Mg powder, MnB powder and Al powder, and a step of internally producing AlB 2 by heat-treating the obtained molded body.
[0014]
DETAILED DESCRIPTION OF THE INVENTION
In the Mg alloy recycling method of the present invention, a mixed powder of Mg powder, MnB powder and Al powder is pressure-molded, and the resulting molded body is heat-treated to internally produce AlB 2 . The internal production of AlB 2 is typically performed by the following reaction.
[0015]
2MnB + Al → 2Mn + AlB 2 (A)
It can be said that the heat-treated molded body is in a state of a particle-dispersed metal matrix composite in which AlB 2 intermetallic compound particles are dispersed in a metal matrix composed of Mg particles, Mn particles, and Al particles.
[0016]
Next, when the AlB 2 -containing molded body obtained above is added to the molten Mg alloy, the metal matrix composed of Mg particles, Mn particles and Al particles is dissolved in the molten metal and reacts with the molten metal as follows.
[0017]
Mn + 6Al + Fe → (FeMn) Al 6 (B)
Thereby, Fe in the Mg alloy is fixed as an intermetallic compound (FeMn) Al 6 and is removed from the molten metal by precipitation separation.
[0018]
At the same time, the AlB 2 particles are dispersed in the molten metal as the metal matrix is dissolved in the molten metal. The internally generated AlB 2 particles are fine particles of submicron to 1 μm and act as a large number of fine solidification nuclei to produce a fine cast structure.
[0019]
As described above, according to the present invention, removal of the Fe content in the Mg alloy and refinement of the cast structure can be performed simultaneously.
[0020]
In addition, in the present invention, since no harmful additive such as hexachloroethane is used as in the prior art, there is no problem from the viewpoint of environmental protection.
[0021]
Note that Mg, which is a component of the molded body, is not involved in any of the reactions (A) and (B). However, when the molded body after heat treatment is added to the molten Mg, Mg is an indispensable component for ensuring the wettability of the molded body and realizing the dissolution of the metal matrix and the dispersion of AlB 2 particles in the molten metal. It is an ingredient.
[0022]
The compounding ratio of the MnB powder and the Al powder constituting the compact is the stoichiometric ratio of Al and B corresponding to the reaction (A) (atomic ratio: Al: B = 1: 2) and the reaction (B ) And the stoichiometric ratio of Mn and Al (Mn: Al = 1: 6 in atomic ratio) corresponding to the standard). The mixing ratio of the Mg powder can be set to an amount sufficient to ensure wettability between the compact and the molten Mg alloy. Summarizing these conditions, the reaction formulas (A) and (B) can be expressed as (A ′) and (B ′) below.
[0023]
αMg + 2MnB + 13Al → αMg + 2Mn + 12Al + AlB 2 (A ′)
2Mn + 12Al + 2Fe → 2 (FeMn) Al 6 (B ′)
Here, each coefficient corresponds to the blending ratio of the green compact powder, and the coefficient α of Mg is generally a large numerical value (blending ratio) of several tens or more.
[0024]
【Example】
The Mg alloy was recycled under the following conditions and procedures.
[0025]
First, Mg powder, MnB powder, and Al powder were weighed so as to have the blending ratio shown in Table 1, and mixed for 30 minutes in a V-type powder mixer.
[0026]
[Table 1]
The obtained mixed powder was pressure-molded at a molding pressure of 7 ton / cm 2 to prepare a cylindrical molded body (φ30 mm, 20 g / piece).
[0028]
This molded body was heat-treated at each temperature shown in Table 2 for 1 hour in an Ar atmosphere.
[0029]
[Table 2]
Mg alloy scrap having the composition shown in Table 3 was melted to form a molten Mg alloy.
[0031]
[Table 3]
2000 g of the molten Mg alloy was maintained at 750 ° C., and the molded body after each heat treatment was added in the addition amount shown in Table 2.
[0033]
The molten metal to which the compact was added was cast under the following conditions.
[0034]
[Casting conditions]
Casting method: Gravity casting mold: JIS No. 4 boat mold mold preheating temperature: 100 ° C
Molten metal temperature during addition: 750 ° C
Melting temperature during casting: 750 ° C
Table 2 shows the results of analysis of Fe content and measurement of crystal grain size for each of the obtained castings.
[0035]
The Fe content was 0.014 mass% in Experiment Nos. 1 to 3 where heat treatment of the compact was performed at 800 ° C. with respect to 0.014 mass% of the raw material scrap, which was equivalent to the raw material scrap. In Experiment Nos. 4 to 9 where the heat treatment of the body was performed at 1000 ° C. or 1200 ° C., it was 0.004 mass%, which was significantly reduced. In either case, the effect of the amount added was not observed. In addition, it confirmed that it was equivalent to a raw material scrap in the case of no molded object addition. FIG. 1 shows the Fe content of the cast product in comparison with Experiment Nos. 4 to 9 in which the Fe removal effect by addition was obtained and Experiment No. 10 without addition.
[0036]
The crystal grain size was 300 μm in Experiment No. 1 to 3 in which heat treatment of the compact was performed at 800 ° C., compared to 300 μm in the case of no additive added, and was equivalent to Experiment No. 10 in which the additive was not added. However, in Experiment Nos. 4 to 9 in which the heat treatment of the molded body was performed at 1000 ° C. or 1200 ° C., it was 50 to 200 μm, and a clear refining effect was recognized. Furthermore, Experiments Nos. 4 to 6 with a heat treatment temperature of 1000 ° C. had a greater effect of miniaturization than Experiments Nos. 7 to 9 with a heat treatment temperature of 1200 ° C.
[0037]
The above results can be interpreted as follows.
[0038]
At 800 ° C., neither of the reactions (A) and (B) occurs. Therefore, neither the effect of refining by the product AlB 2 of the reaction (A) nor the effect of removing Fe by the reaction (B) can be obtained.
[0039]
Since both reaction (A) and (B) occur at 1000 ° C. and 1200 ° C., both the effect of atomization by the product AlB 2 of reaction (A) and the effect of removing Fe by reaction (B) are obtained. Also, in 1000 ° C. grain refining effect is small 1200 ° C. relative to the reaction in addition to the generation of AlB 2 by (A) and also occurs generation of AlB 12 by the following reaction (C), of that much AlB 2 There is little production amount. Since AlB 12 produced by heat treatment at 1200 ° C. does not function as a solidification nucleus, it does not contribute to fine graining, and the fine graining effect is reduced by the amount of production of AlB 2 having a fine graining action.
[0040]
αMg + 12MnB + 13Al → αMg + 12Mn + 12Al + AlB 12 (C)
In the Al—B binary system, AlB 2 is generated at 660 ° C. or higher and AlB 12 is generated at 975 ° C. or higher. However, in the Mg alloy as a multi-component system on the premise of a large amount of Mg, each of the above generations It is thought that the temperature has shifted to the high temperature side.
[0041]
【The invention's effect】
As described above, according to the present invention, the Mg alloy recycling method, recycling agent, and recycling agent that can simultaneously achieve the removal of the Fe content and the refinement of the cast structure without using an additive harmful to the environment. A manufacturing method is provided.
[Brief description of the drawings]
FIG. 1 is a graph showing a comparison of Fe content when a recycling process according to the present invention is performed and when a recycling process is not performed.
Claims (3)
得られた成形体を熱処理することにより該成形体内にＡｌＢ２を内部生成させる工程、および
得られたＡｌＢ２含有成形体をＭｇ合金溶湯に添加する工程
を含むことを特徴とするＭｇ合金のリサイクル方法。A step of pressure-molding a mixed powder of Mg powder, MnB powder and Al powder,
Recycling of Mg alloy characterized by including a step of internally producing AlB 2 in the molded body by heat-treating the obtained molded body, and a step of adding the obtained AlB 2 -containing molded body to a molten Mg alloy Method.
得られた成形体を熱処理することにより該成形体内にＡｌＢ２を内部生成させる工程
を含むことを特徴とするＭｇ合金のリサイクル剤の製造方法。A Mg alloy comprising: a step of pressure-forming a mixed powder of Mg powder, MnB powder and Al powder; and a step of internally producing AlB 2 by heat-treating the obtained molded body. Manufacturing method of recycling agent.
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| JP2002100374A JP3903829B2 (en) | 2002-04-02 | 2002-04-02 | Mg alloy recycling method, recycling agent, and manufacturing method of recycling agent |
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| JP2002100374A JP3903829B2 (en) | 2002-04-02 | 2002-04-02 | Mg alloy recycling method, recycling agent, and manufacturing method of recycling agent |
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| JP3903829B2 true JP3903829B2 (en) | 2007-04-11 |
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