JP6513530B2 - Deoxidation method of Ti-Si alloy - Google Patents
Deoxidation method of Ti-Si alloy Download PDFInfo
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- JP6513530B2 JP6513530B2 JP2015169144A JP2015169144A JP6513530B2 JP 6513530 B2 JP6513530 B2 JP 6513530B2 JP 2015169144 A JP2015169144 A JP 2015169144A JP 2015169144 A JP2015169144 A JP 2015169144A JP 6513530 B2 JP6513530 B2 JP 6513530B2
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- 239000000956 alloy Substances 0.000 title claims description 64
- 229910045601 alloy Inorganic materials 0.000 title claims description 61
- 229910004339 Ti-Si Inorganic materials 0.000 title claims description 38
- 229910010978 Ti—Si Inorganic materials 0.000 title claims description 38
- 238000000034 method Methods 0.000 title claims description 27
- 239000001301 oxygen Substances 0.000 claims description 58
- 229910052760 oxygen Inorganic materials 0.000 claims description 58
- 239000002994 raw material Substances 0.000 claims description 57
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 53
- 238000002844 melting Methods 0.000 claims description 39
- 230000008018 melting Effects 0.000 claims description 39
- 239000000463 material Substances 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910004356 Ti Raw Inorganic materials 0.000 description 17
- 229910001069 Ti alloy Inorganic materials 0.000 description 9
- 239000000203 mixture Substances 0.000 description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 6
- 229910052802 copper Inorganic materials 0.000 description 6
- 239000010949 copper Substances 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 3
- 238000010894 electron beam technology Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 238000011109 contamination Methods 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010891 electric arc Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 1
- 238000011978 dissolution method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- -1 low-grade sponge Ti Chemical compound 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Description
本発明は、酸素を合計で０．１質量％以上含有するＴｉ原料およびＳｉ原料、或いはＴｉ原料およびＳｉ原料を用いて作製した酸素を０．１質量％以上含有するＴｉ−Ｓｉ系合金を、原材料として、低酸素Ｔｉ−Ｓｉ系合金を製造するＴｉ−Ｓｉ系合金の脱酸方法に関するものである。 The present invention is a Ti raw material and Si raw material containing 0.1 mass% or more of oxygen in total, or a Ti—Si based alloy containing 0.1 mass% or more of oxygen produced using Ti raw material and Si raw material, The present invention relates to a method of deoxidizing a Ti—Si based alloy for producing a low oxygen Ti—Si based alloy as a raw material.
近年、航空機や自動車向けの金属素材としてＴｉ合金の需要が高まりつつある。活性金属であるＴｉを主成分とするＴｉ合金を製造する際には、溶解中の酸素による汚染を防ぐ必要があり、従来から真空アーク溶解法（ＶＡＲ）、電子ビーム溶解法（ＥＢ）、プラズマアーク溶解法（ＰＡＭ）、真空誘導溶解法（ＶＩＭ）、水冷銅式誘導溶解法（ＣＣＩＭ）などの溶解法が採用されてきた。 In recent years, the demand for Ti alloys as metal materials for aircrafts and automobiles is increasing. When producing a Ti alloy mainly composed of Ti, which is an active metal, it is necessary to prevent contamination by oxygen during melting, and conventionally, vacuum arc melting (VAR), electron beam melting (EB), plasma Dissolution methods such as arc melting (PAM), vacuum induction melting (VIM), water cooled copper induction melting (CCIM) have been employed.
上記した溶解法の中でも、ＶＡＲ、ＥＢ、ＶＩＭといった溶解法は真空雰囲気下で合金の溶解を行う溶解法であり、このような溶解法を採用した場合、合金元素だけではなく、Ｔｉについても溶解中に揮発してしまいロスを生じることになる。つまり、これら溶解法を採用した場合は工業プロセスにおいて、Ｔｉ合金を目標の組成に制御することが極めて困難であり、その結果、製造コストの増加を招くことにもつながっているのが現状である。 Among the above-mentioned melting methods, the melting methods such as VAR, EB and VIM are melting methods in which the alloy is melted in a vacuum atmosphere, and when such a melting method is adopted, not only alloy elements but also Ti is melted. It will volatilize inside and will cause losses. That is, when these melting methods are employed, it is extremely difficult to control the Ti alloy to a target composition in an industrial process, and as a result, it is also currently linked to causing an increase in manufacturing cost. .
また、酸素含有量が少ないＴｉ合金を溶製するためには、酸素含有量が少ない高品位なＴｉ材料を用いてＴｉ合金を製造することが有効であるが、高品位なＴｉ材料は、高価格であり、特に近年は高騰する傾向にあるため、酸素含有量が例えば０．１質量％以上と多いが、高品位なＴｉ材料より価格が安いスポンジＴｉ、スクラップ原料、ルチル鉱石（ＴｉＯ２）などの比較的低品位なＴｉ材料を用いて酸素濃度が低いＴｉ合金を製造したいというニーズが日々高まっている。 Also, in order to melt a Ti alloy with a low oxygen content, it is effective to use a high quality Ti material with a low oxygen content to produce a Ti alloy, but a high quality Ti material is It is a price, and in particular it tends to soar in recent years, so although the oxygen content is as high as, for example, 0.1% by mass, sponge Ti, scrap raw material, rutile ore (TiO 2 ) whose price is lower than high grade Ti materials. There is a growing need to manufacture Ti alloys with low oxygen concentration using relatively low-grade Ti materials such as.
Ｔｉは活性金属であり、溶解する雰囲気中に存在する酸素との結合力が極めて強いため、溶解中に外部から取り込まれる酸素を低減し、いかに汚染を防ぐかという対策が従来からなされていた。しかし、一度Ｔｉ中に固溶した酸素を除去することは容易ではなく、その取り組み自体が少ないのが現状である。 Since Ti is an active metal and has a very strong bonding force with oxygen present in the dissolving atmosphere, measures have been conventionally taken to reduce the oxygen taken from the outside during the dissolution and to prevent contamination. However, it is not easy to remove oxygen once dissolved in Ti, and the current situation is that the effort itself is small.
このような、Ｔｉ合金などのＴｉの脱酸方法に関する提案は、いくつかは既に存在するが、Ｓｉを脱酸剤として用いたＴｉの脱酸方法としては、特許文献１に記載された提案がある。 Although some proposals for the deoxidation method of Ti such as Ti alloy already exist, the proposal described in Patent Document 1 is a deoxidization method of Ti using Si as a deoxidizer. is there.
この提案は、酸素を含有するＴｉ材料を、Ａｌ或いはＳｉを単独でもしくは組み合わせて添加した状態で電子ビーム溶解して、酸素をＡｌ或いはＳｉの酸化物として気相脱酸しようというものである。特に、実施例３には、Ｓｉを単独で添加して脱酸する方法が記載されており、酸素濃度が０．０５重量％まで除去することができたと記載されている。 This proposal is to dissolve the oxygen-containing Ti material by electron beam in the state where Al or Si is added singly or in combination, and try to deoxidize oxygen as an oxide of Al or Si. In particular, Example 3 describes a method of deoxidizing by adding Si alone, and it is described that the oxygen concentration could be removed up to 0.05% by weight.
しかしながら、特許文献１に記載されたＴｉの脱酸方法は、電子ビーム溶解法（ＥＢ）を採用した脱酸方法であり、前記したような高真空雰囲気での溶解であるため、ＳｉのみならずＴｉの揮発ロスも同時に発生するため、ＴｉおよびＳｉを追加添加する必要があり、製造コストの増加を招くことにもつながってしまう。また、Ｓｉの方がＴｉより蒸気圧が高いため、溶解の際に合金の組成に変化が生じ、Ｔｉ合金を目標の組成に制御することが極めて困難な方法である。 However, the deoxidizing method of Ti described in Patent Document 1 is a deoxidizing method employing electron beam melting (EB), and since it is dissolution in the high vacuum atmosphere as described above, not only Si but also Since volatilization loss of Ti also occurs simultaneously, additional addition of Ti and Si is required, which leads to an increase in manufacturing cost. In addition, since Si has a higher vapor pressure than Ti, the composition of the alloy changes upon melting, and it is an extremely difficult method to control the Ti alloy to a target composition.
本発明は、上記従来の問題を解決せんとしてなされたもので、酸素含有量が高い低品位なＴｉ材料を用いて、酸素含有量が低いＴｉ−Ｓｉ系合金を、目標の組成で、しかも、大気圧に近い圧力下で容易に製造することができるＴｉ−Ｓｉ系合金の脱酸方法を提供することを課題とするものである。 The present invention has been made to solve the above-mentioned conventional problems, and using a low-grade Ti material having a high oxygen content, a Ti-Si alloy having a low oxygen content and a target composition. It is an object of the present invention to provide a method for deoxidizing a Ti—Si alloy which can be easily manufactured under a pressure close to the atmospheric pressure.
本発明のＴｉ−Ｓｉ系合金の脱酸方法は、酸素を合計で０．１質量％以上含有するＴｉ原料およびＳｉ原料、或いはＴｉ原料およびＳｉ原料を用いて作製した酸素を０．１質量％以上含有するＴｉ−Ｓｉ系合金を、原材料として、Ｔｉを主成分とする低酸素Ｔｉ−Ｓｉ系合金を製造するにあたり、前記原材料のＳｉの含有量を３０質量％以上４０質量％以下とし、４．７×１０4Ｐａ〜１．１×１０5Ｐａの圧力下において、前記原材料をアーク溶解により溶解し、その後、保持することによって、低酸素Ｔｉ−Ｓｉ系合金を製造することを特徴とする。
The deoxidation method of the Ti-Si alloy according to the present invention comprises 0.1 mass% of oxygen produced by using Ti raw material and Si raw material, or Ti raw material and Si raw material containing 0.1 mass% or more of oxygen in total When manufacturing a low-oxygen Ti-Si alloy containing Ti as a main component by using the Ti-Si alloy containing the above as a raw material, the content of Si in the raw material is set to 30 mass% or more and 40 mass% or less , 4 . A low oxygen Ti-Si based alloy is produced by melting the raw material by arc melting under a pressure of 7 × 10 4 Pa to 1.1 × 10 5 Pa and then holding it. .
本発明のＴｉ−Ｓｉ系合金の脱酸方法によると、酸素含有量が高い低品位なＴｉ材料を用いて、酸素含有量が原材料より低いＴｉ−Ｓｉ系合金を、ＳｉおよびＴｉの揮発が殆どなく目標の組成で、しかも高真空雰囲気としなくても大気圧に近い圧力下で容易に製造することができる。 According to the deoxidation method of the Ti-Si alloy of the present invention, a Ti-Si alloy having a lower oxygen content than that of the raw material is used with low volatilization of Si and Ti, using a low-grade Ti material having a high oxygen content. It can be easily manufactured at a pressure close to the atmospheric pressure without the target composition and without the high vacuum atmosphere.
本発明者らは、低品位なスポンジＴｉ、スクラップ原料や、ルチル鉱石（ＴｉＯ２）などの酸素を多く含有する低品位なＴｉ材料を用いて、低酸素Ｔｉ合金を、目標の組成で、しかも高真空雰囲気としなくても大気圧に近い圧力下で容易に製造することができる脱酸方法を見出すため、鋭意検討を行った。 The present inventors use low-grade Ti alloy with a target composition and a low-grade Ti material containing a large amount of oxygen such as low-grade sponge Ti, scrap raw materials, and rutile ore (TiO 2 ). The present inventors diligently studied to find a deacidification method which can be easily manufactured under a pressure close to the atmospheric pressure without using a high vacuum atmosphere.
本発明者らは、合金元素に用いる元素としてＳｉに着目した。その結果、合金中のＳｉ濃度が２０質量％以上になると脱酸反応が進行し、低品位なＴｉ材料を用いて作製したＴｉ−Ｓｉ系合金であっても、Ｓｉを２０質量％以上含有するＴｉ−Ｓｉ系合金であれば、高真空雰囲気下でなくとも大気圧に近い圧力下で、ＳｉやＴｉの揮発ロスがなく目標の組成の低酸素Ｔｉ−Ｓｉ系合金を容易に製造できることを見出し、本発明を完成させるに至った。 The present inventors focused on Si as an element used as an alloy element. As a result, when the Si concentration in the alloy reaches 20% by mass or more, the deoxidation reaction proceeds, and even in the case of a Ti—Si-based alloy manufactured using a low grade Ti material, 20% by mass or more of Si is contained. It is found that a Ti-Si alloy can easily produce a low-oxygen Ti-Si alloy having a target composition without volatilization loss of Si or Ti under a pressure close to the atmospheric pressure even if it is not in a high vacuum atmosphere. The present invention has been completed.
以下、本発明を実施形態に基づいて更に詳細に説明する。 Hereinafter, the present invention will be described in more detail based on the embodiments.
本発明のＴｉ−Ｓｉ系合金の脱酸方法は、酸素を合計で０．１質量％以上含有するＴｉ原料およびＳｉ原料、或いはＴｉ原料およびＳｉ原料を用いて作製した酸素を０．１質量％以上含有するＴｉ−Ｓｉ系合金を、原材料として、低酸素Ｔｉ−Ｓｉ系合金を製造するにあたり、原材料のＳｉの含有量を２０質量％以上とし、大気圧に近い４．７×１０４Ｐａ〜１．１×１０５Ｐａの圧力下において、前記原材料を、アーク溶解により溶解し、その後、保持することによって、Ｓｉの含有量を実質的に低下させることなく酸素含有量を低下させて、低酸素Ｔｉ−Ｓｉ系合金を製造する方法である。 The deoxidation method of the Ti-Si alloy according to the present invention comprises 0.1 mass% of oxygen produced by using Ti raw material and Si raw material, or Ti raw material and Si raw material containing 0.1 mass% or more of oxygen in total When producing a low oxygen Ti-Si alloy by using the Ti-Si alloy containing the above as a raw material, the content of Si of the raw material is made 20 mass% or more, and 4.7 × 10 4 Pa which is close to atmospheric pressure The raw material is melted by arc melting under a pressure of 1.1 × 10 5 Pa, and then held to reduce the oxygen content without substantially reducing the content of Si, thereby reducing the content. This is a method of producing an oxygen Ti-Si based alloy.
本発明では、前記Ｔｉ原料としては、低品位なスポンジＴｉ、スクラップ原料や、ルチル鉱石（ＴｉＯ２）などを用いるが、Ｔｉ原料およびＳｉ原料を原材料とする場合のＳｉ原料の添加方法としては、図１に示すような、Ｓｉ原料をＴｉ原料で予め挟み込んで水冷銅容器内へ投入し、溶解を開始するサンドイッチ法、図２に示すように、水冷銅容器内に先にＴｉ原料を投入して溶解した後に、Ｔｉシートで包んだＳｉをＴｉ融体内に投入する投入法などを採用することができる。 In the present invention, low-grade sponge Ti, scrap raw material, rutile ore (TiO 2 ), etc. are used as the Ti raw material, but as a method of adding Si raw material when using Ti raw material and Si raw material as raw materials, As shown in FIG. 1, a Si raw material is sandwiched in advance by a Ti raw material and introduced into a water-cooled copper container, and a sandwich method for starting dissolution, as shown in FIG. It is possible to employ an injection method in which Si wrapped in a Ti sheet is introduced into the Ti melt after melting.
本発明が、Ｔｉ−Ｓｉ系合金の作製に、低品位なスポンジＴｉ、スクラップ原料や、ルチル鉱石（ＴｉＯ２）などの酸素含有量が多いＴｉ原料を用いる理由は、これらＴｉ原料が廉価であり調達し易いからである。 The reason why the present invention uses Ti raw materials having high oxygen content such as low grade sponge Ti, scrap raw materials, and rutile ore (TiO 2 ) for producing Ti-Si based alloys is that these Ti raw materials are inexpensive. It is easy to procure.
これらＴｉ原料およびＳｉ原料よりなる合金材料、或いはこれらＴｉ原料およびＳｉ原料を用いて作製したＴｉ−Ｓｉ系合金の、酸素含有量を０．１質量％以上とした理由は、酸素含有量が０．１質量％未満であれば、酸素の含有量は僅かであり脱酸自体が必要ないからである。尚、本発明では、酸素の含有量の上限は規定しないが、前記合金材料などに実際に含有される酸素含有量の上限は、多くても５．０質量％程度であると考えられる。 The oxygen content of the alloy material made of these Ti raw material and Si raw material, or the Ti-Si based alloy produced using these Ti raw material and Si raw material, is 0.1 mass% or more, the oxygen content is 0 If it is less than 1% by mass, the content of oxygen is small and deoxidation itself is not necessary. In the present invention, although the upper limit of the content of oxygen is not defined, it is considered that the upper limit of the oxygen content actually contained in the alloy material and the like is at most about 5.0 mass%.
原材料のＳｉの含有量、すなわち、Ｔｉ原料およびＳｉ原料よりなる合金材料、或いはこれらＴｉ原料およびＳｉ原料を用いて作製したＴｉ−Ｓｉ系合金の、Ｓｉの含有量を、２０質量％以上とした理由は、原材料中のＳｉの含有量が２０質量％以上であれば、Ｔｉ−Ｓｉ系合金の脱酸が進行するからである。 The content of Si in the raw material, that is, the content of Si in the alloy material made of the Ti raw material and the Si raw material, or the Ti-Si based alloy manufactured using the Ti raw material and the Si raw material, is 20 mass% or more The reason is that if the content of Si in the raw material is 20% by mass or more, deoxidation of the Ti-Si alloy proceeds.
この脱酸反応は液相において発現する現象で、Ｔｉ−Ｓｉ系合金の場合は、ＳｉＯＸの蒸気圧が、純Ｔｉの蒸気圧より高くなると脱酸反応が進行する。Ｔｉ−Ｓｉ系合金のＳｉ含有量が２０質量％以上であれば、Ｔｉ−Ｓｉ系合金が溶解する概ね２４００Ｋ以上の温度で、ＳｉＯＸの蒸気圧が十分高くなり、脱酸反応が進行する。尚、ＳｉＯＸの蒸気圧は高温になるほど高くなり脱酸反応はより進行する。その温度の上限はＴｉの蒸気圧が５．６×１０３Ｐａとなる３０００Ｋ程度である。 This deoxidation reaction is a phenomenon that occurs in the liquid phase, and in the case of a Ti—Si alloy, the deoxidation reaction proceeds when the vapor pressure of SiO X becomes higher than the vapor pressure of pure Ti. If the Si content of the Ti-Si alloy is 20% by mass or more, the vapor pressure of SiO X becomes sufficiently high at a temperature of about 2400 K or more at which the Ti-Si alloy dissolves, and the deoxidation reaction proceeds. As the vapor pressure of SiO x becomes higher as the temperature becomes higher, the deoxidation reaction progresses more. The upper limit of the temperature is about 3000 K at which the vapor pressure of Ti is 5.6 × 10 3 Pa.
原材料中のＳｉの含有量の更に好ましい下限は３０質量％であり、原材料中のＳｉの含有量が３０質量％以上であれば、脱酸の進行はより顕著になり、Ｔｉ−Ｓｉ系合金の酸素含有量は確実に０．１質量％を下回る。尚、本発明では、原材料中のＳｉの含有量の上限は特に規定しないが、実際上の原材料中のＳｉの含有量の上限は４０質量％程度である。Ｔｉ−Ｓｉ系合金はＳｉ以外の他の合金元素や酸素などの不純物も含有するので、合金元素であるＳｉの含有量が多くなり過ぎるとＴｉの割合が少なくなりＴｉ−Ｓｉ系合金ということができなくなる。 A further preferable lower limit of the content of Si in the raw material is 30% by mass, and if the content of Si in the raw material is 30% by mass or more, the progress of deoxidation becomes more remarkable, and the Ti-Si alloy The oxygen content is certainly below 0.1% by weight. In the present invention, the upper limit of the content of Si in the raw material is not particularly defined, but the upper limit of the content of Si in the actual raw material is about 40% by mass. Since the Ti-Si alloy also contains impurities such as other alloy elements and oxygen other than Si, if the content of Si which is an alloy element becomes too large, the proportion of Ti decreases and it is called a Ti-Si alloy. become unable.
本発明では原材料を溶解するにあたりアーク溶解を採用するが、アーク溶解には、プラズマアーク溶解が含まれることは勿論である。また、原材料のアーク溶解は、４．７×１０４Ｐａ（３５０Ｔｏｒｒ）〜１．１×１０５Ｐａ（８３０Ｔｏｒｒ）の圧力下で、Ａｒガス、Ｈｅガスなどを用いた不活性ガス雰囲気下で行う。 In the present invention, arc melting is employed to melt the raw materials, but arc melting naturally includes plasma arc melting. In addition, arc melting of the raw material is performed under a pressure of 4.7 × 10 4 Pa (350 Torr) to 1.1 × 10 5 Pa (830 Torr) under an inert gas atmosphere using Ar gas, He gas, etc. .
圧力の下限を４．７×１０４Ｐａ（３５０Ｔｏｒｒ）とした理由は、この圧力以上であれば、溶解プロセス中にアーク放電が可能であり、また、ＳｉやＴｉの揮発ロスを低減できるからである。好ましい下限は、より安定なアーク放電が可能となる５．３×１０４Ｐａ（４００Ｔｏｒｒ）である。また上限を１．１×１０５Ｐａ（８３０Ｔｏｒｒ）とした理由は、この圧力がアーク溶解時の到達炉内圧力の上限と考えられるからであり、好ましい上限は一般的なアーク溶解における溶解条件である１．０×１０５Ｐａ（７６０Ｔｏｒｒ）である。 The lower limit of the pressure is set to 4.7 × 10 4 Pa (350 Torr) because if it is higher than this pressure, arc discharge can be performed during the melting process, and the volatilization loss of Si and Ti can be reduced. is there. The preferred lower limit is 5.3 × 10 4 Pa (400 Torr) which enables more stable arc discharge. The reason why the upper limit is set to 1.1 × 10 5 Pa (830 Torr) is that this pressure is considered to be the upper limit of the pressure in the reaching furnace at the time of arc melting, and the preferable upper limit is the melting conditions in general arc melting It is 1.0 × 10 5 Pa (760 Torr).
尚、本発明のＴｉ−Ｓｉ系合金の脱酸方法は、Ｓｉの含有量を低下させることなく酸素濃度を低下させて、低酸素Ｔｉ−Ｓｉ系合金を製造する方法であるとしているが、先に記載したように、Ｓｉの含有量は極僅かに低下しても構わない。許容できるＳｉの含有量の低下率は５．０％以下であり、本発明であれば、Ｓｉの含有量の低下率を５．０％以下とすることができる。 The deoxidation method of the Ti-Si alloy of the present invention is a method of producing a low-oxygen Ti-Si alloy by reducing the oxygen concentration without reducing the content of Si. As described in, the content of Si may be slightly reduced. The allowable reduction rate of the Si content is 5.0% or less, and in the present invention, the reduction rate of the Si content can be 5.0% or less.
以下、実施例を挙げて本発明をより具体的に説明するが、本発明はもとより下記実施例によって制限を受けるものではなく、本発明の趣旨に適合し得る範囲で適宜変更を加えて実施することも可能であり、それらは何れも本発明の技術的範囲に含まれる。 EXAMPLES Hereinafter, the present invention will be more specifically described by way of examples. However, the present invention is of course not limited by the following examples, and the present invention is implemented by adding appropriate changes as long as they can conform to the spirit of the present invention. It is also possible that they are all included in the technical scope of the present invention.
（Ｔｉ−Ｓｉ系合金中のＳｉ含有量と溶解後の酸素含有量の関係）
Ｔｉ−Ｓｉ系合金中のＳｉの含有量が、アーク溶解後の到達酸素含有量に及ぼす影響を調べるために、初期酸素含有量が１．６質量％と０．１質量％に調整された高酸素Ｔｉ−Ｓｉ系合金試料を作製した。
(Relationship between Si content in Ti-Si alloy and oxygen content after melting)
In order to investigate the influence of the Si content in the Ti-Si alloy on the final oxygen content after arc melting, the initial oxygen content was adjusted to 1.6 mass% and 0.1 mass%. An oxygen Ti-Si based alloy sample was prepared.
酸素含有量が１．６質量％の合金試料については、Ｓｉの含有量が３質量％、５質量％、９．１質量％、１７質量％、２３質量％、３０質量％の合金試料をそれぞれ準備した。これら合金試料を用いて、７６０Ｔｏｒｒの圧力下において、Ａｒガスを用いた不活性ガス雰囲気下で、アーク溶解を実施した。表１に各合金試料のアーク溶解前後の酸素含有量を、図３に各合金試料のアーク溶解前後の質量変化を、それぞれ示す。 With respect to an alloy sample having an oxygen content of 1.6% by mass, the alloy samples having a content of Si of 3% by mass, 5% by mass, 9.1% by mass, 17% by mass, 23% by mass, and 30% by mass, respectively Got ready. Using these alloy samples, arc melting was carried out under an inert gas atmosphere using Ar gas under a pressure of 760 Torr. Table 1 shows the oxygen content of each alloy sample before and after arc melting, and FIG. 3 shows the mass change before and after arc melting of each alloy sample.
表１によると、Ｓｉの含有量が３質量％、５質量％、９．１質量％、１７質量％の合金試料では、アーク溶解後の到達酸素含有量が、初期酸素含有量の１．６０６質量％からあまり下がっておらず脱酸が進行していないのに対し、Ｓｉの含有量が２３質量％の合金試料では、アーク溶解後の到達酸素含有量が確実に下がっており、脱酸が進行していることが分かる。また、Ｓｉの含有量が３０質量％の合金試料では、アーク溶解後の到達酸素含有量は大きく低下しており、脱酸の進行はより顕著である。 According to Table 1, in the alloy samples having a Si content of 3% by mass, 5% by mass, 9.1% by mass, and 17% by mass, the final oxygen content after arc melting is the initial oxygen content of 1.606. In the alloy sample with a Si content of 23% by mass, the final oxygen content after arc melting has definitely decreased, whereas the amount of deoxidization has not decreased so much from the mass%, and the deoxidation is not You can see that it is in progress. Further, in the alloy sample having a Si content of 30% by mass, the final oxygen content after arc melting is greatly reduced, and the progress of deoxidation is more remarkable.
図３に各合金試料のアーク溶解前後の質量変化を示すが、殆ど質量変化は確認できず、ＳｉおよびＴｉの揮発が殆どないことが分かる。 Although the mass change before and behind arc melting of each alloy sample is shown in FIG. 3, almost no mass change can be confirmed, and it can be seen that there is almost no volatilization of Si and Ti.
また、酸素含有量が０．１質量％の合金試料については、Ｓｉの含有量（添加量）が３質量％、１０質量％、３０質量％の合金試料をそれぞれ準備した。これら合金試料を用いて、７６０Ｔｏｒｒの圧力下において、Ａｒガスを用いた不活性ガス雰囲気下で、アーク溶解を実施した。表２に各合金試料のアーク溶解前後の酸素含有量を示す。 Moreover, about the alloy sample whose oxygen content is 0.1 mass%, 3 mass%, 10 mass%, and 30 mass% alloy samples of Si content (addition amount) were prepared, respectively. Using these alloy samples, arc melting was carried out under an inert gas atmosphere using Ar gas under a pressure of 760 Torr. Table 2 shows the oxygen content before and after arc melting of each alloy sample.
表２によると、Ｓｉの含有量が３質量％、１０質量％の合金試料では、アーク溶解後の到達酸素含有量が、初期酸素含有量の０．１０３８質量％から殆ど下がっておらず脱酸が進行していないのに対し、Ｓｉの含有量が３０質量％の合金試料では、アーク溶解後の到達酸素含有量は大きく低下しており、脱酸が確実に進行している。 According to Table 2, in the alloy sample having a Si content of 3% by mass and 10% by mass, the ultimate oxygen content after arc melting is hardly reduced from 0.1038% by mass of the initial oxygen content, and deoxidation In the alloy sample of which the content of Si is 30% by mass, the final oxygen content after arc melting is greatly reduced while deoxidation is progressing reliably.
Claims (1)
前記原材料のＳｉの含有量を３０質量％以上４０質量％以下とし、
４．７×１０4Ｐａ〜１．１×１０5Ｐａの圧力下において、前記原材料をアーク溶解により溶解し、その後、保持することによって、低酸素Ｔｉ−Ｓｉ系合金を製造することを特徴とするＴｉ−Ｓｉ系合金の脱酸方法。 Ti material and Si material containing oxygen in total more than 0.1 wt%, or Ti-Si-based alloy containing oxygen more than 0.1 wt% produced using a Ti material and Si source, as raw materials, Ti In producing low-oxygen Ti-Si based alloys containing
The content of Si in the raw material is 30 % by mass or more and 40% by mass or less ,
The raw material is melted by arc melting under a pressure of 4.7 × 10 4 Pa to 1.1 × 10 5 Pa, and then held to manufacture a low-oxygen Ti—Si-based alloy. Method for deoxidizing a Ti-Si alloy.
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