JPH02221337A - Method for pulverizing ti-nb alloy - Google Patents
Method for pulverizing ti-nb alloyInfo
- Publication number
- JPH02221337A JPH02221337A JP1040617A JP4061789A JPH02221337A JP H02221337 A JPH02221337 A JP H02221337A JP 1040617 A JP1040617 A JP 1040617A JP 4061789 A JP4061789 A JP 4061789A JP H02221337 A JPH02221337 A JP H02221337A
- Authority
- JP
- Japan
- Prior art keywords
- alloy
- hydrogen
- ingot
- pulverizing
- pulverized
- 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.)
- Pending
Links
- 229910001257 Nb alloy Inorganic materials 0.000 title claims abstract description 26
- 238000010298 pulverizing process Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 title claims description 7
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001257 hydrogen Substances 0.000 claims abstract description 14
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 14
- 229910045601 alloy Inorganic materials 0.000 abstract description 8
- 239000000956 alloy Substances 0.000 abstract description 8
- 239000004570 mortar (masonry) Substances 0.000 abstract description 5
- 229910003074 TiCl4 Inorganic materials 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 150000004678 hydrides Chemical class 0.000 abstract description 3
- 238000011084 recovery Methods 0.000 abstract description 3
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 abstract description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- 229910019804 NbCl5 Inorganic materials 0.000 abstract 1
- YHBDIEWMOMLKOO-UHFFFAOYSA-I pentachloroniobium Chemical compound Cl[Nb](Cl)(Cl)(Cl)Cl YHBDIEWMOMLKOO-UHFFFAOYSA-I 0.000 abstract 1
- 239000000843 powder Substances 0.000 description 8
- 238000005660 chlorination reaction Methods 0.000 description 7
- 150000001805 chlorine compounds Chemical class 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- -1 TlC14 and NbC1a Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010894 electron beam technology Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000010079 rubber tapping Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910001281 superconducting alloy Inorganic materials 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
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明はＴｌ−Ｎｂ合金の粉砕方法であって、超伝導用
に使用するＴｉ−Ｎｂ棒加工のスクラップを粉砕し、Ｔ
ｉ、 Ｎｂの回収を容易ならしめることを目的とするも
のである。Detailed Description of the Invention [Industrial Application Field] The present invention is a method for pulverizing Tl-Nb alloy, which involves pulverizing scraps from processed Ti-Nb bars used for superconductivity, and pulverizing Tl-Nb alloy.
The purpose is to facilitate the recovery of Nb.
［発明の背景］
現在Ｔｉ−Ｎｂ合金（Ｔｉ 約４６胃１９ｇ）は、超
伝導用合金として最も広く使用されているが、合金組成
および元素の均一性が線材の臨界電流に大きく影響する
と言われている。[Background of the Invention] Ti-Nb alloy (approximately 46 grams of Ti and 19 grams of Ti) is currently the most widely used superconducting alloy, but it is said that the alloy composition and uniformity of elements greatly affect the critical current of the wire. ing.
一般に超伝導用に使用するＴｉ−Ｎｂ合金は、該合金イ
ンゴットを真空中でアーク溶解またはエレクトロンビー
ム溶解等で溶解してＴｉ−Ｎｂ棒加工または複合加工さ
れて銅等のマトリックス中にＴｉ−Ｎｂ細線として埋め
込まれて使用されている。Generally, Ti-Nb alloys used for superconducting are melted by arc melting or electron beam melting in vacuum, and processed into Ti-Nb rods or composite processed to form Ti-Nb in a matrix of copper or the like. It is embedded and used as a thin line.
前述Ｔｉ−Ｎｂインゴットを棒加工または複合加工する
際約２０％のスクラップが発生するが、ＴｉもＮｂも高
価な金属であるため回収する必要があり、該スクラップ
を一部再溶解して回収するかまたは高級鋼の添加用とし
て使用されているに過ぎない。Approximately 20% of the scrap is generated when the aforementioned Ti-Nb ingot is processed into bars or composite processed, but since both Ti and Nb are expensive metals, it is necessary to recover them, and some of the scrap is remelted and recovered. Or it is only used as an additive to high-grade steel.
［従来の技術］ 従来、前記のごときＴｉ−ＮｂスクラップからＴＩ。[Conventional technology] Conventionally, TI was produced from Ti-Nb scrap as described above.
Ｎｂを分離して回収することが考えられており、その手
段として塩素化による分離が提案されているが、今のと
ころ工業的に実施されるに至っていない。It has been considered to separate and recover Nb, and separation by chlorination has been proposed as a means for this, but so far it has not been implemented industrially.
すなわち、前記塩素化によるＴＩ、 Ｎｂの分離、回収
の方法はＴｉ−Ｎｂ合金を塩素化してＴｌＣ１４および
ＮＭ：ｌｓとした後、蒸留してＴｉＣｌ４およびＮｂＣ
１１に分離した後、ＮａまたはＭｇ等で還元してＴＩま
たはＮｂを分離、回収するものである。That is, the method for separating and recovering TI and Nb by chlorination is to chlorinate a Ti-Nb alloy to obtain TlC14 and NM:ls, and then distill it to obtain TiCl4 and NbC.
After separating into 11, TI or Nb is separated and recovered by reduction with Na or Mg or the like.
ｃ本発明が解決しようとする課題］
しかし、Ｔｉ−Ｎｂインゴットまたは棒加ニスクラップ
のものの塩素化は反応性が悪く、そのためには粉末状と
する必要がある。そのため、Ｔｌ−Ｎｂインゴット等を
旋盤で削りた切り粉等とする方法が考えられるが、塩素
化にはさらに微粉末とする必要があり、微粉末処理が困
難であるばかりか製造効率が悪い。c) Problems to be Solved by the Present Invention] However, chlorination of Ti-Nb ingots or bar scraps has poor reactivity, and for this purpose it is necessary to form them into powder. Therefore, a method can be considered in which Tl--Nb ingots are ground into chips using a lathe, but chlorination requires further pulverization, which not only makes pulverization difficult but also reduces manufacturing efficiency.
本発明は超伝導用に使用するＴｉ−Ｎｂ合金スクラップ
から塩素化によってＴｉ、 Ｎｂを回収するに当たり、
Ｔｌ−Ｎｂ合金を簡単に微粉砕できる方法を提供するこ
とにある。The present invention recovers Ti and Nb from Ti-Nb alloy scrap used for superconducting by chlorination.
The object of the present invention is to provide a method for easily pulverizing Tl-Nb alloy.
［！！！題を解決するための手段］
本発明はＴｌ−Ｎｂ合金インゴットを真空下で加熱して
水素を吸蔵せしめた後粉砕するＴｌ−Ｎｂ合金の粉砕方
法である。[! ! ! Means for Solving the Problem] The present invention is a method for pulverizing a Tl-Nb alloy, in which a Tl-Nb alloy ingot is heated under vacuum to absorb hydrogen and then pulverized.
Ｔｌ−Ｎｂ合金に水素を吸蔵させるには真空容器内にＴ
ｉ−Ｎｂインゴットないしは棒加工Ｔｌ−Ｎｂのスクラ
ップを挿入し、１０−１〜１Ｇ−’ Ｔｏｒｒに減圧し
つつ容器を２００〜５００℃に加熱し保持する。To make the Tl-Nb alloy absorb hydrogen, add T in the vacuum container.
An i-Nb ingot or a scrap of bar-processed Tl-Nb is inserted, and the container is heated to and held at 200 to 500°C while reducing the pressure to 10-1 to 1 G-' Torr.
次いで前記真空容器を１００〜３００℃に加熱し、水素
ガスを１〜３０ ａｔｍで導入し、保持することによっ
てＴｉ−Ｎｂ合金に水素を吸蔵せしめる。Next, the vacuum container is heated to 100 to 300°C, hydrogen gas is introduced at 1 to 30 atm, and is maintained to cause the Ti-Nb alloy to absorb hydrogen.
水素吸蔵が終了した後、真空容器を室温まで冷却すると
ともに、該真空容器内の水素ガスを除去し、空気を導入
した後Ｔｌ−Ｎｂ水素化物を取り出す。After hydrogen storage is completed, the vacuum vessel is cooled to room temperature, hydrogen gas in the vacuum vessel is removed, air is introduced, and the Tl-Nb hydride is taken out.
水素吸蔵処理されたＴｉ−Ｎｂ水素化物は、当初のイン
ゴットの形態は崩れ一部崩壊した状態であって、乳鉢等
で簡単に粉砕でき微粉（１００メツシユ下）が容易に得
られる。The Ti-Nb hydride subjected to the hydrogen storage treatment is in a state where the original ingot shape is collapsed and partially collapsed, and it can be easily ground in a mortar or the like to easily obtain a fine powder (100 mesh or less).
なお、ここに粉砕されたものは水素ガスを吸蔵している
ため、再び真空容器に挿入し、３００〜８００℃に加熱
しつつ排気すれば簡単に脱水素化したＴｌ−Ｎｂ合金の
粉末が得られる。Since the crushed material absorbs hydrogen gas, dehydrogenated Tl-Nb alloy powder can be easily obtained by inserting it into the vacuum container again and evacuation while heating it to 300 to 800°C. It will be done.
［作用］
本発明は機械的に粉砕困難なＴｉ−Ｎｂ合金に水素を吸
蔵せしめることによって該合金内にクラックを生ぜしめ
ることによって乳鉢等で簡単に粉砕することができる。[Function] The present invention allows a Ti--Nb alloy, which is difficult to crush mechanically, to absorb hydrogen and thereby generate cracks in the alloy, thereby making it possible to easily crush it in a mortar or the like.
従って、水素を吸蔵させ易崩壊性とされたＴｉ−Ｎｂ合
金を乳鉢等で粉砕しこれを脱水素化したものを、前記塩
素化処理によってＴｌＣ１４、ＮｂＣ１ａ等の塩化物と
し、これら塩化物を蒸留によってＴｉＣｌ４およびＮｂ
Ｃｌ５に分離した後、ＮａまたはＭｇで還元することに
よって高収率でＴＩおよびＮｂを回収することができる
。Therefore, a Ti-Nb alloy that has absorbed hydrogen and is easily disintegrated is crushed in a mortar or the like, dehydrogenated, and then subjected to the chlorination treatment to produce chlorides such as TlC14 and NbC1a, and these chlorides are distilled. TiCl4 and Nb by
After separation into Cl5, TI and Nb can be recovered in high yield by reduction with Na or Mg.
［実施例］
Ｔｉ−Ｎｂ合金の丸棒（３φ）１０ｇをステンレス製容
器に挿入し密封した後、３００℃に加熱しつつロータリ
ーポンプで約３０分排気（５Ｘ １Ｏ−２Ｔｏｒｒ）
Ｌ／、その後１５０℃で水素ガス圧を３０ａｔｍにする
まで水素ガスを導入して水素を吸蔵させた。約３時間後
に該合金１ ｍｏ１当たりの水素量（Ｈ／Ｍ）が１．１
５であった。[Example] After inserting 10 g of a Ti-Nb alloy round rod (3φ) into a stainless steel container and sealing it, it was heated to 300°C and evacuated using a rotary pump for about 30 minutes (5X 1O-2 Torr).
After that, hydrogen gas was introduced at 150° C. until the hydrogen gas pressure reached 30 atm to absorb hydrogen. After about 3 hours, the amount of hydrogen per mo1 of the alloy (H/M) was 1.1.
It was 5.
次に、該合金を室温まで冷却し、水素ガスをパージした
後、容器から取り出した。得られたＴｌ−Ｎｂ合金丸棒
は崩壊して丸棒の原形はとどめず、一部２ｍｍ程度の小
塊を含む粉末状であった。The alloy was then cooled to room temperature, purged of hydrogen gas, and then removed from the container. The obtained Tl-Nb alloy round bar collapsed and did not retain its original shape, but was in the form of a powder containing small lumps of about 2 mm in size.
前述小塊を含めこれを乳鉢で軽くたたくことによって全
量１００メツシユ下の微粉末とすることができた。By tapping the powder including the aforementioned small lumps in a mortar, it was possible to make a fine powder with a total amount of less than 100 mesh.
次に、この微粉末を再び真空容器に挿入して約７００℃
に加熱しつつ排気を行ない脱水素化し、Ｔｌ−Ｎｂ合金
の粉末とすることができた。Next, insert this fine powder into the vacuum container again and heat it to about 700°C.
Dehydrogenation was carried out by evacuation while heating to a temperature of 100.degree. C., and a Tl--Nb alloy powder was obtained.
［発明の効果］
以上のごとく本発明は超伝導用として用いられるＴｌ−
Ｎｂ合金を棒加工する際に生ずるスクラップに水素を吸
蔵させることによって粉砕困難なＴｉ−Ｎｂ合金を簡単
に粉砕することができ、従ってＴＩ、 Ｎｂ等の金属を
回収するに当たり塩素化処理等の効率を高め、Ｔｌ−Ｎ
ｂの回収率を向上することができる。[Effects of the Invention] As described above, the present invention provides Tl-
By storing hydrogen in the scrap generated when Nb alloy is processed into bars, it is possible to easily crush the Ti-Nb alloy, which is difficult to crush, thereby increasing the efficiency of chlorination treatment, etc. when recovering metals such as TI and Nb. Tl-N
The recovery rate of b can be improved.
Claims (1)
−Ｎｂ合金のインゴットに水素を吸蔵せしめた後粉砕す
ることを特徴とするＴｉ−Ｎｂ合金の粉砕方法。A Ti-Nb alloy ingot is heated under vacuum and the Ti
- A method for pulverizing a Ti--Nb alloy, which comprises pulverizing an ingot of the Nb alloy after occluding hydrogen therein.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1040617A JPH02221337A (en) | 1989-02-21 | 1989-02-21 | Method for pulverizing ti-nb alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1040617A JPH02221337A (en) | 1989-02-21 | 1989-02-21 | Method for pulverizing ti-nb alloy |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02221337A true JPH02221337A (en) | 1990-09-04 |
Family
ID=12585489
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1040617A Pending JPH02221337A (en) | 1989-02-21 | 1989-02-21 | Method for pulverizing ti-nb alloy |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02221337A (en) |
-
1989
- 1989-02-21 JP JP1040617A patent/JPH02221337A/en active Pending
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