JPH07122105B2 - High-purity, fine-grain metal material manufacturing method - Google Patents
High-purity, fine-grain metal material manufacturing methodInfo
- Publication number
- JPH07122105B2 JPH07122105B2 JP4143491A JP14349192A JPH07122105B2 JP H07122105 B2 JPH07122105 B2 JP H07122105B2 JP 4143491 A JP4143491 A JP 4143491A JP 14349192 A JP14349192 A JP 14349192A JP H07122105 B2 JPH07122105 B2 JP H07122105B2
- Authority
- JP
- Japan
- Prior art keywords
- solid
- metal material
- grain boundaries
- crystal
- fine
- 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
Links
- 239000007769 metal material Substances 0.000 title claims description 64
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- 239000013078 crystal Substances 0.000 claims description 53
- 239000012535 impurity Substances 0.000 claims description 41
- 239000007787 solid Substances 0.000 claims description 31
- 239000011344 liquid material Substances 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 21
- 238000002844 melting Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 13
- 239000002245 particle Substances 0.000 claims description 10
- 239000000919 ceramic Substances 0.000 claims description 8
- 238000005728 strengthening Methods 0.000 claims description 7
- 239000000758 substrate Substances 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 4
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000000155 melt Substances 0.000 claims description 3
- 230000006911 nucleation Effects 0.000 claims description 3
- 238000010899 nucleation Methods 0.000 claims description 3
- 230000003014 reinforcing effect Effects 0.000 claims description 3
- 239000000284 extract Substances 0.000 claims description 2
- 238000007711 solidification Methods 0.000 claims 1
- 230000008023 solidification Effects 0.000 claims 1
- 229910045601 alloy Inorganic materials 0.000 description 13
- 239000000956 alloy Substances 0.000 description 13
- 229910052751 metal Inorganic materials 0.000 description 10
- 239000002184 metal Substances 0.000 description 10
- 239000000047 product Substances 0.000 description 9
- 238000000746 purification Methods 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 6
- ODINCKMPIJJUCX-UHFFFAOYSA-N Calcium oxide Chemical compound [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 4
- 235000012255 calcium oxide Nutrition 0.000 description 4
- 239000000292 calcium oxide Substances 0.000 description 4
- 239000007790 solid phase Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 229910000990 Ni alloy Inorganic materials 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000012265 solid product Substances 0.000 description 3
- 229910000838 Al alloy Inorganic materials 0.000 description 2
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910018140 Al-Sn Inorganic materials 0.000 description 1
- 229910018507 Al—Ni Inorganic materials 0.000 description 1
- 229910018564 Al—Sn Inorganic materials 0.000 description 1
- 229910000967 As alloy Inorganic materials 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000975 Carbon steel Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000881 Cu alloy Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 239000010962 carbon steel Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 238000007429 general method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000013528 metallic particle Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 102220062469 rs786203185 Human genes 0.000 description 1
- 238000009991 scouring Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 238000004857 zone melting Methods 0.000 description 1
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
【０００１】[0001]
【産業上の利用分野】本発明は、高純度金属材料または
微細結晶粒金属材料の製造方法に関するものであり、さ
らに詳しくは、地球生態系に与える影響を少なくするこ
とを考慮して開発し、特に合金を含む各種金属材料の再
生利用のために有効ならしめた高純度・微細結品粒金属
材料の製造方法に関するものである。BACKGROUND OF THE INVENTION The present invention relates to a high-purity metallic material or
The present invention relates to a method for producing a fine-grain metal material , and more specifically, it was developed in consideration of reducing the effect on the global ecosystem, and is particularly effective for the recycling of various metal materials including alloys. and a method for producing a high-purity, fine Hosoyui products grain metal material.
【０００２】[0002]
【従来の技術】現在までの再資源化技術は、地球生態系
に与える影響を殆ど考慮せずに、新材開発に奔走した製
造プロセスを基に、つくられた製品を再利用するため
の、いわば消極的な手法といえる。このような技術開発
だけでは、年々悪化の一途をたどる地球環境への抜本的
な解決にはならない。そこで、材料を製造する前から地
球生態系に与える影響を考慮し、再資源化にも有効な新
しい素材製造プロセスの開発が急務となっている。さら
に、この新しく開発した素材製造プロセスを基に、生態
系負荷軽減化のための環境づくりに積極的に取り組む必
要がある。2. Description of the Related Art Recycling technology up to now has been designed to reuse the products made based on the manufacturing process that has been devoted to the development of new materials, with little consideration given to the impact on the global ecosystem. It can be said that it is a passive method. Such technological development alone cannot provide a drastic solution to the global environment, which is getting worse year by year. Therefore, there is an urgent need to develop a new material manufacturing process that is effective for recycling, considering the effect on the global ecosystem even before manufacturing the material. Furthermore, based on this newly developed material manufacturing process, it is necessary to actively work to create an environment for reducing the ecological load.
【０００３】一方、金属材料の高純度化の方法として
は、従来から、帯溶融精製法、チョコラルスキー法など
があるが、スクラップなどの低品位の金属材料の高純度
化の方法の主流は、エレクトロスラグ・リメルテングな
どの溶湯とスラッグとの化学反応を利用して溶湯中の不
純物質を除去する方法が一般である。しかしながら、こ
の場合においても前述した生態系負荷軽減化について十
分な配慮がなされていない。On the other hand, as a method for highly purifying a metal material, there have been conventionally known a zone melting refining method, a Czochralski method and the like. The mainstream of the method for highly purifying a low grade metal material such as scrap is as follows. A general method is to remove impurities in the molten metal by utilizing a chemical reaction between the molten metal such as electroslag and remelting and the slag. However, even in this case, sufficient consideration has not been given to the reduction of the ecosystem load described above.
【０００４】[0004]
【発明が解決しようとする課題】本発明の技術的課題
は、このような地球生態系に与える影響を考慮した素材
製造プロセスの一つとして、特に合金を含む各種金属材
料の再生利用に適し、半溶融精練と呼ぶことが可能な方
法であって、省エネルギー型で、金属の溶解に際して大
量に発生するＣＯ２を最小限に抑えることが可能な、金
属材料の高純度化及び結晶粒微細化のための方法を提供
することにある。The technical problem to be solved by the present invention is suitable for recycling of various metal materials including alloys, as one of the material manufacturing processes in consideration of the influence on the earth ecosystem. It is a method that can be called semi-melting refining, is an energy-saving method, and is capable of minimizing CO 2 generated in a large amount at the time of melting a metal, and achieving high purification of metal materials and refinement of crystal grains. To provide a way to do so.
【０００５】[0005]
【課題を解決するための手段・作用】上記課題を解決す
るための本発明の第１の高純度金属材料製造方法は、結
晶粒界や固体結晶間隙に不純物質が混入した金属材料、
あるいはそこに微細な非金属物質の強化粒子が混入した
粒子分散強化金属材料を、完全に溶解せずに固液が共存
する半溶融温度まで加熱して、結晶粒界や固体結晶間隙
部分を溶解し、それらの結晶粒界や固体結晶間隙に存在
した不純物質あるいは微細な非金属物質の強化粒子を、
溶解した液状材料と共に排出除去し、残存する金属材料
を圧縮成形することを特徴とするものである。The first high-purity Dokin metal material production method of the present invention for solving the above object, according-effects to an aspect of the metal material impurity substance is mixed in a grain boundary or a solid crystalline gap,
Alternatively, the particle-dispersion-strengthened metallic material, in which fine particles of strengthening non-metallic substances are mixed, is heated to a semi-melting temperature where solid-liquid coexists without completely melting, and crystal grain boundaries and solid crystal gap portions are melted. However, the strengthening particles of impurities or fine non-metallic substances existing in those crystal grain boundaries or solid crystal gaps,
It is characterized in that it is discharged and removed together with the melted liquid material, and the remaining metal material is compression-molded.
【０００６】また、本発明の第２の微細結品粒金属材料
製造方法は、結晶粒界や固体結晶間隙に不純物質が混入
した金属材料を、完全に溶解せずに固液が共存する半溶
融温度まで加熱して、結晶粒界や固体結晶間隙部分を溶
解し、セラミックフィルターによってそれらの結晶粒界
や固体結晶間隙に存在した不純物質を分離除去すると同
時に、溶湯に同時多発的に均質核生成させる基質を提供
して、溶解した液状材料を抽出し、この液状材料の固化
により均質微細なミクロ組織を持つ金属材料を得ること
を特徴とするものである。[0006] The second fine Hosoyui products grain metal material production method of the present invention, a metal material impurity substance is mixed in a grain boundary or a solid crystalline interstitial solid-liquid co-exist without complete dissolution By heating to a semi-melting temperature, the crystal grain boundaries and solid crystal gaps are melted, and the impurities existing in those crystal grain boundaries and solid crystal gaps are separated and removed by a ceramic filter, and at the same time, they are homogeneous in the molten metal at the same time. The present invention is characterized by providing a substrate for nucleation, extracting a melted liquid material, and solidifying the liquid material to obtain a metal material having a homogeneous fine microstructure.
【０００７】さらに具体的に説明すると、本発明の第１
の方法は、金属材料製品の劣化が、その製品の使用期間
中に周囲環境から主に結晶粒界や固体結晶間隙に侵入し
集積する不純物質に起因することに着目し、その不純物
質の集積部分を溶解して、その溶解部分を圧搾、遠心分
離、その他の任意強制分離手段を用いて排出除去するこ
とにより、使用済み製品から再生利用可能な金属材料を
効率的に回収し、あるいはそれと同等の金属材料を対象
として高純度化を行い、しかもそれを省エネルギー型で
金属の溶解に際して大量に発生するＣＯ２を最小限に抑
えながら行い、上記高純度化を達成するものである。ま
た、合金において少量添加されている一部の溶質（例え
ば、アルミニウム合金におけるＭｎやＭｇ）も、不純物
元素として、金属材料における上記結晶粒界や固体結晶
間隙に濃縮された状態で存在しているが、本発明では、
合金成分として本来含まれているこれらの不純物元素を
も、上述した不純物質として分離排出することができ
る。従って、本明細書における不純物質とは、上述した
合金における不純物元素をも包含するものである。More specifically, the first aspect of the present invention will be described.
The method described in (1) focuses on the fact that the deterioration of a metal material product is caused by impurities that infiltrate and accumulate from the ambient environment mainly into the grain boundaries and solid crystal gaps during the use period of the product, and the accumulation of the impurities Dissolve the part, squeeze the melted part, centrifuge
Separation and other optional forced separation means are used for efficient removal of recyclable metal materials from used products, or high purity purification of metal materials equivalent to that is possible. This is an energy-saving type and is performed while minimizing a large amount of CO 2 generated when the metal is melted to achieve the above-described high purification . In addition, some solutes (for example, Mn and Mg in aluminum alloy) that are added in small amounts in the alloy exist as impurity elements in a state of being concentrated in the crystal grain boundaries and solid crystal gaps in the metal material. However, in the present invention,
These impurity elements originally contained as alloy components can also be separated and discharged as the above-mentioned impurities. Therefore, the term “impurity” in this specification includes the impurity elements in the above-mentioned alloy.
【０００８】一方、本発明の第２の方法は、上記不純物
質の排出除去に際して溶解したところの結晶粒界や固体
結品間隙部分の液状材料からフィルター分離可能な不純
物質を除去すると同時に、その結晶粒を微細化しようと
するもので、上記溶解した液状材料をセラミックフィル
ターを通して抽出し、上記セラミックフィルターにより
液状材料中から上記不純物質を分離除去すると同時に、
溶湯に同時多発的に均質核生成させる基質を提供し、こ
の液状材料の固化により均質微細なミクロ組織を持つ金
属材料を得るものである。On the other hand, the second method of the present invention is an impure substance that can be separated from the liquid material in the crystal grain boundaries or the solid product gaps where the impurities are dissolved when the impurities are discharged and removed.
At the same time as removing the substance, it is intended to refine the crystal grains, the molten liquid material is extracted through a ceramic filter, and at the same time the impurities are separated and removed from the liquid material by the ceramic filter,
It provides a substrate for homogeneous nucleation of molten metal at the same time, and solidifies the liquid material to obtain a metallic material having a homogeneous fine microstructure.
【０００９】このように、本発明は、金属材料製品のス
クラップ等、各種製品として使用済みの金属材料、ある
いはそれと同等の各種金属材料を、高純度化及び結晶粒
微細化の対象とするものであり、具体的には、アルミニ
ウム合金、銅合金（粒子分散強化銅）、ニッケル合金、
チタン合金、鉄鋼材料、超合金（ＯＤＳなど）が、処理
の対象として好適であるが、それらに限ることなく、各
種金属材料に適用することができる。As described above, according to the present invention, a metal material that has been used as various products such as scraps of metal material products, or various metal materials equivalent to the metal material, are subjected to high purification and grain refinement. Yes, specifically, aluminum alloy, copper alloy (particle dispersion strengthened copper), nickel alloy,
Titanium alloys, steel materials, and superalloys (such as ODS) are suitable for the treatment, but the present invention is not limited to these and can be applied to various metal materials.
【００１０】上記金属材料は、結晶粒界や固体結晶間隙
に侵入、集積した不純物質を除去して、再生利用可能な
金属材料を効率的に回収するため、完全に溶解せずに、
半溶融温度まで加熱するが、これによって図１に模式的
に示すように、結晶粒界や固体結晶間隙部分が溶解し、
そこに混入、集積していた不純物質が、溶解した液状材
料と共に流動可能な状態になる。同図中、１は粗大な結
晶部分、２は不純物質を濃縮状態で含む液状材料、３は
結晶粒界や固体結晶間隙に侵入集積していた不純物質を
示している。The above metal material does not completely dissolve in order to efficiently collect the recyclable metal material by removing impurities accumulated and entering the crystal grain boundaries and solid crystal gaps.
It is heated to a semi-melting temperature, which melts crystal grain boundaries and solid crystal gaps, as schematically shown in FIG.
Impurities that have been mixed and accumulated there become in a flowable state together with the dissolved liquid material. In the figure, 1 is a coarse crystal part, 2 is a liquid material containing impurities in a concentrated state, and 3 is impurities that have invaded and accumulated in grain boundaries and solid crystal gaps.
【００１１】半溶融の温度は、全容積中に固体が占める
割合（固相率）が４０〜７０％の範囲に対応する温度に
することが必要である。固相率が７０％以上では、部分
溶解した液体領域がまだ固体結品中に分散し、他の液体
とは分断した状態にあるので、固相結晶間隙を通して液
相が流動できない。また、固相率が４０％以下の場合に
は、純粋な固体結晶部分も溶解するので、不純物質を濃
縮状態で効率よく回収できない。It is necessary that the temperature of the semi-melting is a temperature corresponding to the range of the solid content (solid phase ratio) in the total volume of 40 to 70%. When the solid phase ratio is 70% or more, the partially dissolved liquid region is still dispersed in the solid product and is in a state of being separated from other liquids, so that the liquid phase cannot flow through the solid phase crystal gap. Further, when the solid phase ratio is 40% or less, the pure solid crystal part is also dissolved, so that the impurities cannot be efficiently collected in a concentrated state.
【００１２】本発明の第１の方法において、金属材料か
ら不純物質を含む液状材料を排出除去するためには、図
２に例示するように、容器５内に金属材料を収容してピ
ストン状の加圧部材６でそれを圧縮することにより、不
純物質３で汚染された液状材料２を搾り出すようにして
排出除去するが、それによって容器５内に高純度化した
金属材料１ａを得ることができる。また、上述の容器５
内に残存する金属材料１ａは、それを必要な形状に圧縮
成形するが、固体と液体が共存する高い温度領域では、
中間温度や低温の完全な固相単体状態に比べて、固体結
晶の強度が極端に低下するために、結晶の変形や破断・
破砕が容易に起こり、微細結晶粒組織を出現させること
もできる。従って、上記圧縮成形により、高純度化と同
時に結晶粒が微細化された金属材料からなる所期の製品
を得ることができる。[0012] In the first method of the present invention, in order to discharge removing liquid material containing the impure material from metal materials, as illustrated in FIG. 2, and accommodates a metallic material in the vessel 5 pin
The liquid material 2 contaminated with the impurities 3 is squeezed out and removed by compressing it with the stone- shaped pressure member 6, and thereby the container 5 is highly purified. The metal material 1a can be obtained. In addition, the above-mentioned container 5
The metal material 1a remaining inside is compression molded into a required shape, but in a high temperature region where solid and liquid coexist,
Compared to the complete solid state at intermediate and low temperatures, the strength of solid crystals is extremely reduced, which may cause crystal deformation or fracture.
Fracture occurs readily, causing the appearance of fine grain structure
You can also Therefore, the compression molding described above is equivalent to the purification.
Sometimes it is possible to obtain a desired product made of a metal material in which crystal grains are refined.
【００１３】本発明の第１の方法は、上述した結晶粒界
等に不純物質が混入した使用済み金属材料や、前記不純
物元素を含んでいる合金等に適用することができるが、
さらに、粉末治金法やコンポキャスト法等で製造され
て、結晶粒界や固体結晶間隙に微細な非金属物質の強化
粒子を混入させている粒子分散強化金属材料の再生利用
にも適用することができる。The first method of the present invention can be applied to the above-mentioned used metal material in which impurities are mixed in the crystal grain boundaries, alloys containing the above-mentioned impurity elements, etc.
Furthermore, it can be applied to the recycling of particle-dispersion-strengthened metallic materials that are manufactured by powder metallurgy or compocasting methods and have fine non-metallic reinforcing particles mixed in the grain boundaries and solid crystal gaps. You can
【００１４】これらの金属材料では、微細な非金属物質
の強化粒子の多くが不純物質と共に結晶粒界や固体結品
間隙に存在するため、前記再生用の金属材料と同様に、
固体と液体が共存する半溶融温度まで加熱すると、ま
ず、固体結晶間隙あるいは結晶粒界が液体状態になるの
で、その中に存在する微細非金属粒子等は液状材料中に
懸垂した状態で、その液状材料と共に流動する。従っ
て、その金属材料を圧縮することにより、非金属物質の
強化粒子及び不純物質が混入した液状材料を排出除去
し、不純物質を強化粒子と共に排出した金属材料を得る
ことができ、その残存する金属材料を圧縮成形すること
によって、上述した場合と同様に、高純度化された金属
材料を得ることができる。In these metal materials, most of the reinforcing particles of the fine non-metallic substance are present in the crystal grain boundaries and the solid product gaps together with the impurities. Therefore, like the above-mentioned metal material for reproduction,
When heated to a semi-melting temperature where a solid and a liquid coexist, first, the solid crystal gaps or crystal grain boundaries are in a liquid state, so the fine non-metallic particles and the like present therein are suspended in the liquid material, It flows with the liquid material. Therefore, by compressing the metal material, it is possible to discharge and remove the liquid material in which the strengthening particles of the non-metal substance and the impurities are mixed, and to obtain the metal material in which the impurities are discharged together with the strengthening particles. By compression molding the material, a highly purified metal material can be obtained as in the case described above.
【００１５】一方、本発明の第２の方法においては、図
２によって先に説明したように、容器５内において半溶
融状態の金属材料を圧縮し、強化用の微細な非金属物質
粒子や、合金における前記不純物元素、その他の不純物
質３を含む液状材料２を排出するに際し、それをセラミ
ックフィルター７に通すことにより、液状材料中から上
記不純物質３等を除去すると同時に、その結晶粒の微細
化のために有効に作用させる。即ち、上記セラミックフ
ィルター７により、溶解した液状材料２中から不純物質
３を分離除去して高純度化した液状材料２ａを抽出する
と同時に、溶湯に同時多発的に均質核生成させる基質
（ｓｕｂｓｔｒａｔｅ）を提供し、この液状材料の固化
により均質微細なミクロ組織を持つ金属材料を得るもの
である。上記セラミックフィルターとしては、ＣａＯな
どの溶湯中の不純物との化学反応が活発に生じ易いもの
が適し、このようなフィルターを用いた場合には、溶解
した液状材料中に固溶している不純物をも吸い取って溶
融物を清浄化するので、結果的に濾過した後の液状材料
はそれに固溶している不純物も除去されることを確かめ
ている。 On the other hand, in the second method of the present invention, as described above with reference to FIG. 2, the semi-molten metal material is compressed in the container 5 and fine non-metallic substance particles for strengthening, When the liquid material 2 containing the impurity element and other impurities 3 in the alloy is discharged, the liquid material 2 is passed through a ceramic filter 7 to remove the impurities 3 and the like from the liquid material and, at the same time, to finely crystallize the crystal grains. It effectively acts for conversion. That is, the ceramic filter 7 extracts the highly purified liquid material 2a by separating and removing the impurities 3 from the melted liquid material 2, and at the same time, forms a substrate (substrate) for simultaneously and homogeneously nucleating the molten metal. The present invention is to provide a metal material having a uniform fine microstructure by solidifying this liquid material. As the above-mentioned ceramic filter, one that is likely to undergo a chemical reaction actively with impurities in the molten metal such as CaO is suitable.
The impurities dissolved in the liquid material
Liquid material after filtering, resulting in cleaning of the melt
Make sure that the impurities dissolved in it are also removed
ing.
【００１６】このような方法によって前記金属材料の高
純度化または結晶粒の微細化を行うと、再生しようとす
る金属材料を完全に溶解する必要がなく、そのため完全
に再溶解する場合に大量に発生するＣＯ２を、最小限に
抑えることができ、省エネルギーによる金属材料の高純
度化と結晶粒微細化を実現することができる。When the metal material is highly purified or the crystal grains are refined by such a method, it is not necessary to completely dissolve the metal material to be regenerated, and therefore, when completely remelting, a large amount is required. The generated CO 2 can be suppressed to a minimum, and high purification of metal material and miniaturization of crystal grains can be realized by energy saving.
【００１７】[0017]
【実施例】以下に本発明の実施例を示す。Ａｌ−５０ｗ
ｔ％Ｓｎ合金供試材料を黒鉛の鋳型に入れて、その鋳型
を収容したチャンバー内を真空排気（１０ −５ ｔｏｒ
ｒ）したうえで、半溶融温度領域に等温保持し、等温保
持開始２時間後に、供試材の上表面に接しているピスト
ン状部材（図２の加圧部材６に相当）によって、押出速
度１〜１０ｍｍ／ｈｒで加圧し、結晶間隙に発生した不
純物質が濃縮された液体を、Ｓ３５Ｃ炭素鋼製フィルタ
ーを通して流下させることにより除去し、高純度アルミ
ニウム材料を製造した。 結果を表１乃至表４に示す。表
１はＡｌ−５０ｗｔ％Ｓｎ合金の高速処理の結果を、表
２は、その際に流下した液体材料の分析結果を示すもの
であり、表３は、同低速処理の結果を、表４は、その際
に流下した液体材料の分析結果を示すものである。 EXAMPLES Examples of the present invention will be shown below. Al-50w
Put the t% Sn alloy test material in a graphite mold and
The chamber containing the gas is evacuated (10 −5 torr).
r) and then keep isothermally in the semi-melting temperature range
2 hours after the start of holding, the piste in contact with the upper surface of the test material
The extrusion speed can be increased by the ring-shaped member (corresponding to the pressure member 6 in FIG. 2).
When pressure is applied at a rate of 1 to 10 mm / hr, the
S35C carbon steel filter for liquids containing pure substances
High-purity aluminum
A Ni material was manufactured. The results are shown in Tables 1 to 4. table
Table 1 shows the results of high-speed treatment of Al-50 wt% Sn alloy.
2 shows the analysis result of the liquid material flowing down at that time
Table 3 shows the result of the low speed processing, and Table 4 shows the result at that time.
It shows the analysis results of the liquid material that has flowed down.
【００１８】[0018]
【表１】 [Table 1]
【００１９】[0019]
【表２】 [Table 2]
【００２０】[0020]
【表３】 [Table 3]
【００２１】[0021]
【表４】 [Table 4]
【００２２】 また、各種Ａｌ−Ｎｉ合金を供試材料と
し、上記Ａｌ−Ｓｎ合金の場合と同様であるが、結晶間
隙に発生した不純物質が濃縮された液体を、９９％アル
ミナからなるフィルターを通して流下させた場合の結果
を表５及び表６に示す。表５はＡｌ−２ｗｔ％Ｎｉ合金
の場合の結果を、表６はＡｌ−１ｗｔ％Ｎｉ合金の場合
の結果を、図７は上記表５及び表６の場合を含む各種実
験後の純度と回収重量についての測定結果を示すもので
ある。 Further, the various Al-Ni alloy test materials
However, the same as in the case of the Al-Sn alloy, but between the crystals
The liquid containing the impurities generated in the gap was
Table 5 and Table 6 show the results when the particles were made to flow through a filter composed of Mina . Table 5 shows Al-2wt% Ni alloy
Table 6 shows the results in the case of Al-1 wt% Ni alloy
Fig. 7 shows various results including the cases of Tables 5 and 6 above.
It shows the measurement results of the purity and the recovered weight after the test.
is there.
【００２３】[0023]
【表５】 [Table 5]
【００２４】[0024]
【表６】 [Table 6]
【００２５】[0025]
【表７】 [Table 7]
【００２６】さらに、不純物質の除去及び均質微細のミ
クロ組織の出現を確認するために、Ａｌ−４８ｗｔ％Ｔ
ｉ合金をカルシア坩堝に入れて真空溶解し、一定温度に
保持後、実質的に図２に示すような状態で、上方よりピ
ストン状の加圧部材６で溶湯に接する面を２ｍｍ／ｍｉ
ｎの速度で押し込み、坩堝底部のポーラスなＣａＯフィ
ルターを通して上記組成の合金を流出させた。その結
果、同組成合金の普通鋳造合金には見られない均質微細
のミクロ組織を出現させることができ、かつ、ＣａＯフ
ィルターにより不純物質が除去された金属材料を製造で
きた。図３の図面代用写真は、得られた合金の組織を示
すもので、その結晶粒が微細化されていることがわか
る。 Furthermore, the removal and homogeneous fine impurities substance Mi
To confirm the appearance of black tissue, Al-48 wt% T
was vacuum melted putting i alloy calcia crucible, after holding at a constant temperature, substantially in a state shown in FIG. 2, peak from above
The surface contacting the molten metal is 2 mm / mi with the stone- shaped pressure member 6.
It was pushed in at a speed of n to let out the alloy having the above composition through a porous CaO filter at the bottom of the crucible. As a result, a homogeneous fine microstructure, which is not found in ordinary cast alloys of the same composition, can be made to appear, and a metallic material from which impurities have been removed by the CaO filter can be manufactured. The drawing-substitute photograph of FIG. 3 shows the structure of the obtained alloy, and it can be seen that the crystal grains are refined.
【００２７】[0027]
【発明の効果】以上に詳述した本発明の方法によれば、
特に金属材料の再生利用に適し、半溶融精練と呼ぶこと
が可能な方法であって、省エネルギー型で、金属の溶解
に際して大量に発生するＣＯ２を最小限に抑えることが
可能な、金属材料の高純度化及び結晶粒微細化のための
方法を提供することができる。According to the method of the present invention detailed above,
It is particularly suitable for recycling metal materials, and is a method that can be called semi-melt scouring, which is an energy-saving method and is capable of minimizing a large amount of CO 2 generated during melting of metals. A method for high purification and grain refinement can be provided.
【図１】本発明に基づいて金属材料を固液が共存する半
溶融温度まで加熱した状態を示す説明図である。FIG. 1 is an explanatory view showing a state in which a metal material is heated to a semi-melting temperature at which a solid liquid coexists according to the present invention.
【図２】本発明の方法の実施態様を説明するための断面
図である。FIG. 2 is a cross-sectional view for explaining an embodiment of the method of the present invention.
【図３】本発明の方法によって得られた合金の組織を示
す図面代用写真である。FIG. 3 is a drawing-substituting photograph showing the structure of an alloy obtained by the method of the present invention.
１ 粗大な結晶部分、 １ａ 金属材料、 ２ 不純物質を含む液状材料部分、 ２ａ 液状材料、 ３ 不純物質、 ７ セラミックス・フィルター。 1 coarse crystal part, 1a metallic material, 2 liquid material part containing impurities, 2a liquid material, 3 impurities, 7 ceramics filter.
Claims (3)
した金属材料を、完全に溶解せずに固液が共存する半溶
融温度まで加熱して、結晶粒界や固体結晶間隙部分を溶
解し、それらの結品粒界や固体結晶間隙に存在した不純
物質を、溶解した液状材料と共に排出除去し、残存する
金属材料を圧縮成形することを特徴とする高純度金属材
料の製造方法。1. A metal material, in which impurities are mixed in the crystal grain boundaries or solid crystal gaps, is heated to a semi-melting temperature at which solid liquids coexist without being completely dissolved, and thereby the crystal grain boundaries or solid crystal gap portions are removed. lysed and the impure material that was present in their binding products grain boundaries and solid crystals gap, and discharged and removed together with the dissolved liquid material, the production of high-purity Dokin metal material, which comprises compression-molding a metallic material remaining Method.
質の強化粒子が混入した粒子分散強化金属材料を、完全
に溶解せずに固液が共存する半溶融温度まで加熱して、
結晶粒界や固体結晶間隙部分を溶解し、それらの結晶粒
界や固体結晶間隙に存在した微細な非金属物質の強化粒
子を、溶解した液状材料と共に排出除去し、残存する金
属材料を圧縮成形することを特徴とする高純度金属材料
の製造方法。2. A particle-dispersed strengthening metal material in which reinforcing particles of fine non-metallic substances are mixed in crystal grain boundaries or solid crystal gaps is heated to a semi-melting temperature at which solid-liquid coexists without completely melting,
Dissolves crystal grain boundaries and solid crystal gaps, discharges and removes fine non-metallic substance strengthening particles that existed in these crystal grain boundaries and solid crystal gaps together with the dissolved liquid material, and compresses the remaining metal material. method for producing a high purity Dokin metal material, characterized by.
した金属材料を、完全に溶解せずに固液が共存する半溶
融温度まで加熱して、結晶粒界や固体結晶間隙部分を溶
解し、セラミックフィルターによってそれらの結晶粒界
や固体結晶間隙に存在した不純物質を分離除去すると同
時に、溶湯に同時多発的に均質核生成させる基質を提供
して、溶解した液状材料を抽出し、この液状材料の固化
により均質微細なミクロ組織を持つ金属材料を得ること
を特徴とする微細結晶粒金属材料の製造方法。3. A metal material in which impurities are mixed in crystal grain boundaries or solid crystal gaps is heated to a semi-melting temperature at which solid liquid coexists without being completely melted, so that crystal grain boundaries or solid crystal gap portions are removed. Dissolve and separate and remove impurities existing in those crystal grain boundaries and solid crystal gaps by a ceramic filter, and at the same time provide a substrate for homogeneous nucleation in the melt simultaneously and extract the melted liquid material, method for producing a fine fine grain metallic material you and obtaining a metal material having a homogeneous fine microstructure by solidification of the liquid material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4143491A JPH07122105B2 (en) | 1992-05-08 | 1992-05-08 | High-purity, fine-grain metal material manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4143491A JPH07122105B2 (en) | 1992-05-08 | 1992-05-08 | High-purity, fine-grain metal material manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05311260A JPH05311260A (en) | 1993-11-22 |
| JPH07122105B2 true JPH07122105B2 (en) | 1995-12-25 |
Family
ID=15339949
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4143491A Expired - Lifetime JPH07122105B2 (en) | 1992-05-08 | 1992-05-08 | High-purity, fine-grain metal material manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH07122105B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7834803B2 (en) * | 2024-06-03 | 2026-03-24 | 株式会社神戸製鋼所 | Method for producing aluminum raw materials, method for producing aluminum material, and compression apparatus |
-
1992
- 1992-05-08 JP JP4143491A patent/JPH07122105B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05311260A (en) | 1993-11-22 |
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