JP2003053419A - Method for drawing iridium of iridium alloy wire - Google Patents
Method for drawing iridium of iridium alloy wireInfo
- Publication number
- JP2003053419A JP2003053419A JP2001251241A JP2001251241A JP2003053419A JP 2003053419 A JP2003053419 A JP 2003053419A JP 2001251241 A JP2001251241 A JP 2001251241A JP 2001251241 A JP2001251241 A JP 2001251241A JP 2003053419 A JP2003053419 A JP 2003053419A
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- Prior art keywords
- iridium
- die
- wire
- temperature
- alloy wire
- Prior art date
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Classifications
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- 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
- Y02P10/25—Process efficiency
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- Metal Extraction Processes (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、イリジウム又はイ
リジウム合金からなる線材を引抜き加工により断面積を
減少させる加工方法に関する。詳しくは欠陥のない高品
質のイリジウム又はイリジウム合金線材を効率的に製造
するための製造方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a working method for reducing the cross-sectional area of a wire made of iridium or an iridium alloy by drawing. More particularly, it relates to a manufacturing method for efficiently manufacturing a high-quality iridium or iridium alloy wire rod having no defects.
【０００２】[0002]
【従来の技術】イリジウム及びイリジウムを主成分とす
る合金（イリジウム−白金合金、イリジウム−ロジウム
合金等）は高融点、高硬度及び高耐食性という性質か
ら、従来からるつぼ、不溶性電極として利用されてい
る。近年では、その耐酸化特性及び電気特性についても
特異な性質を有することが注目されており、今後その他
の分野での利用も検討されている。近年のイリジウム合
金の利用例としては、自動車等の内燃機関用点火プラグ
の電極、ドットプリンターのピン先等がある。このよう
にイリジウム合金の適用範囲が広がっているのは、例え
ば、点火プラグの電極についていえば、イリジウムが白
金族金属の中でも融点が高いために揮発損失が少なく耐
火花酸化特性に優れているということに基づくものであ
る。2. Description of the Related Art Iridium and alloys containing iridium as a main component (iridium-platinum alloy, iridium-rhodium alloy, etc.) have been conventionally used as crucibles and insoluble electrodes because of their high melting point, high hardness and high corrosion resistance. . In recent years, it has been noted that it has unique properties with respect to its oxidation resistance and electrical properties, and its use in other fields is also being studied in the future. Examples of recent applications of iridium alloys include electrodes for spark plugs for internal combustion engines of automobiles, pin tips of dot printers, and the like. In this way, the range of application of iridium alloys is expanding, for example, in the case of spark plug electrodes, because iridium has a high melting point among platinum group metals, there is little volatilization loss and excellent spark oxidation resistance. It is based on that.
【０００３】このような点火プラグを電極等の用途に適
用するには、細径の線材とし、これを適宜の長さに切断
しているが、線材の製造は鍛造加工、圧延加工等により
製造される線材（棒材）からこれを引抜き加工すること
によりなされている。In order to apply such a spark plug to a use such as an electrode, a wire having a small diameter is cut and cut into an appropriate length. The wire is manufactured by forging, rolling or the like. It is made by drawing this from a wire rod (bar material).
【０００４】イリジウム及びイリジウム合金は、高融点
材料（イリジウムの融点は２４００℃以上である）であ
る上に、常温では比較的脆く加工が困難であることか
ら、熱間での加工が適用されるのが通常である。そし
て、このことは引抜き加工においても同様であり、従来
のイリジウム合金の引抜き加工は１３００℃前後の高温
での引抜き加工がなされている。図６は、従来のイリジ
ウム合金線材の引抜き加工工程を概略図示したものであ
る。被加工材であるイリジウム線材１は加工前に潤滑剤
６を塗布され、バーナー８の火炎９にて加熱される。加
熱された線材はダイス３を通過してより線径の小さい線
材となる。そして、加工目的の線材の線径をより小さく
したい場合にはこの工程を繰り返すこととなる。この従
来の引抜き加工工程は、バーナーによる加熱という簡便
な加熱手段により線材を所定の加工温度とすることがで
きることから広く行なわれている方法である。Since iridium and iridium alloys are high melting point materials (the melting point of iridium is 2400 ° C. or higher) and are relatively brittle at room temperature and difficult to process, hot working is applied. Is normal. This also applies to the drawing process, and the conventional iridium alloy drawing process is carried out at a high temperature of about 1300 ° C. FIG. 6 schematically shows a conventional iridium alloy wire rod drawing process. The iridium wire 1 which is the work piece is coated with the lubricant 6 before being processed and heated by the flame 9 of the burner 8. The heated wire rod passes through the die 3 to become a wire rod having a smaller wire diameter. Then, when it is desired to reduce the wire diameter of the wire rod for processing, this step is repeated. This conventional drawing process is a widely used method because the wire can be heated to a predetermined processing temperature by a simple heating means such as heating with a burner.
【０００５】[0005]
【発明が解決しようとする課題】ところで、上記のよう
にして製造されるイリジウム合金線材には、傷や皺、割
れ、組織的不均一といった欠陥がないことや線径が一定
であること等が求められるが、この品質基準は近年ます
ます厳しいものとなっている。例えば、近年の自動車用
エンジンの高性能化には目覚しいものがあるが、エンジ
ンの高性能化には信頼性の高い点火プラグは不可欠であ
る。そして、割れを有する電極はたとえその欠陥が微小
なものであっても、放電特性の不安定化の要因となり、
その寿命を予想以上に短期化することが考えられ、その
信頼性を低下させることとなることから、欠陥の全くな
い線材が求められるのである。The iridium alloy wire rod manufactured as described above is free from defects such as scratches, wrinkles, cracks, and structural nonuniformity, and has a constant wire diameter. Although required, this quality standard has become increasingly stringent in recent years. For example, although there are remarkable improvements in the performance of automobile engines in recent years, a highly reliable spark plug is indispensable for improving the performance of the engine. And, even if the electrode having a crack has a minute defect, it becomes a factor of destabilizing the discharge characteristics,
The life of the wire may be shortened more than expected, and the reliability of the wire may be reduced. Therefore, a wire having no defects is required.
【０００６】かかる要求に対し、従来の製造条件、製造
方法は、線材の断面積減少という本来の目的においては
ほぼ満足させることができるが、その品質においては必
ずしも十分なものとはいえない。特に、今後要求される
従来以上に高い品質基準を考慮すれば、欠陥のない高精
度の成形加工技術の確立が求められるといえる。[0006] In order to meet such requirements, the conventional manufacturing conditions and manufacturing methods can be almost satisfied for the original purpose of reducing the cross-sectional area of the wire, but their quality is not always sufficient. In particular, it can be said that establishment of a high-precision molding process technology without defects is required in consideration of higher quality standards than required in the future.
【０００７】そこで、本発明はイリジウム又はイリジウ
ム合金よりなる線材を引抜き加工する方法において、よ
り効率的で且つ欠陥のない高品質の線材を成型加工する
ことができる方法を提供することを目的とする。[0007] Therefore, an object of the present invention is to provide a method for drawing a wire made of iridium or an iridium alloy, which is more efficient and can form a high-quality wire without defects. .
【０００８】[0008]
【課題を解決するための手段】本発明者は、かかる課題
を解決すべく、まず、イリジウムを熱間で引抜き加工す
る際における加工条件の最適化を図ることとした。一般
に、材料加工の条件としては、加工温度、加工率（引抜
き加工においては断面減少率）の選定が重要となる。こ
の点、イリジウムの場合、上述したように融点、常温で
の靭性を考慮して、従来は加工温度を高温としている。
そこで、本発明者等は、まずイリジウムの引抜き加工に
おいて加工温度による被加工材の状態変化につき検討し
次の知見を得た。In order to solve the above problems, the present inventor first decided to optimize the processing conditions when hot drawing iridium. Generally, as conditions for material processing, selection of processing temperature and processing rate (area reduction rate in drawing) is important. In this respect, in the case of iridium, the processing temperature is conventionally set to a high temperature in consideration of the melting point and the toughness at room temperature as described above.
Therefore, the inventors of the present invention first examined the change in the state of the work material depending on the processing temperature in the iridium drawing process, and obtained the following findings.
【０００９】図１は、イリジウム合金の引抜き加工を常
温及び高温で引抜き加工したときの破断状況を示すもの
である、まず、低温（常温）加工した場合、図１（ａ）
のようにイリジウム合金線材には破断が生じるが、この
ときの破断はダイス内で生じる。この常温における破断
発生の要因は、ダイス内における線材の塑性加工抵抗が
ダイス出口付近の線材の引張力よりも大きくなることに
よるものである。この場合、線材を加熱して線材を軟化
させることで塑性加工抵抗を減少させ破断の発生を防止
することができる。FIG. 1 shows the fracture state of the iridium alloy drawn at room temperature and high temperature. First, when the low temperature (normal temperature) processing is performed, FIG.
As described above, the iridium alloy wire rod is fractured, but the fracture at this time occurs in the die. The cause of fracture at room temperature is that the plastic working resistance of the wire in the die becomes larger than the tensile force of the wire near the die exit. In this case, by heating the wire to soften the wire, the plastic working resistance can be reduced and the occurrence of breakage can be prevented.
【００１０】一方、加工温度を高温とした場合において
も線材の破断は生じ得る。このときの破断は図１（ｂ）
のように、ダイス内部ではなくダイス通過後において発
生するものであるが、これは、加熱による加工抵抗が低
下することでダイス内での破断は生じないものの、ダイ
ス通過後の材料強度が引張力よりも小さくなっているこ
とによるものである。そして、この材料強度低下の要因
としては、高温に加熱することで材料に再結晶が生じ、
結晶粒成長及び粒界への不純物の偏析等の要因により粒
界強度が低下し脆化する結果、材料全体の強度が低下す
るためと考えられる。On the other hand, even if the working temperature is high, the wire may be broken. The fracture at this time is shown in Fig. 1 (b).
As described above, it occurs not through the inside of the die but after passing through the die.However, this does not cause breakage in the die due to the reduction in processing resistance due to heating, but the material strength after passing through the die is the tensile force. It is because it is smaller than. And as a factor of this material strength reduction, recrystallization occurs in the material by heating to a high temperature,
It is considered that the grain boundary strength is reduced and embrittlement is caused by factors such as crystal grain growth and segregation of impurities in the grain boundaries, and as a result, the strength of the entire material is reduced.
【００１１】以上の低温、高温での引抜き加工時の挙動
を勘案すれば、イリジウム合金の引抜き加工において
は、加熱が必要ではあるが、その温度は再結晶の生じな
い範囲で行なう必要がある。即ち、イリジウム合金の加
工可能な温度には所定の範囲（加工可能領域）が存在
し、この範囲を形成する上限及び下限が存在するものと
考えられる。Considering the above-mentioned behavior at the time of drawing at a low temperature and a high temperature, heating is necessary in the drawing of an iridium alloy, but the temperature must be within a range where recrystallization does not occur. That is, it is considered that the processable temperature of the iridium alloy has a predetermined range (processable region), and there is an upper limit and a lower limit forming this range.
【００１２】他方、この加工可能な温度範囲は、一律に
定められるものではなく、加工率により変動するものと
考えられる。即ち、加工率の上昇により加工抵抗は高く
なることから、図２で示すように加工温度の下限値は加
工率の上昇にともない高温側にシフトすると考えられる
（図２の線）。一方、上限値についていえば、加工率
の上昇により再結晶温度が低下し、これに関連して上限
値も低下するものと考えられる（図２の線）。On the other hand, the temperature range in which processing is possible is not fixed uniformly, but it is considered that it varies depending on the processing rate. That is, since the working resistance increases as the working rate increases, it is considered that the lower limit of the working temperature shifts to the high temperature side as the working rate rises, as shown in FIG. 2 (line in FIG. 2). On the other hand, regarding the upper limit value, it is considered that the recrystallization temperature decreases due to the increase in the processing rate, and the upper limit value also decreases in connection with this (the line in FIG. 2).
【００１３】このように、イリジウム線材の引き抜き加
工においては、加工率に応じた加工可能な温度範囲が存
在し、これは変動するものである。一方、この加工可能
領域とは、単に破断を生じさせることなく加工できるか
を示すに過ぎず、欠陥のない高品質の線材を加工できる
範囲を示すものではない。つまり、下限値付近の加工温
度では加工抵抗と材料強度の関係により破断は生じない
が微小クラックが生じる領域が存在すると考えられる。
また、上限値付近の加工温度においては、上記した再結
晶は材料内部のみならず表面にも現れることから材料表
面の荒れの要因となる。従って、加工温度の上限値につ
いては加工率の変化により変化する再結晶温度も考慮す
る必要がある。従って、加工可能領域の中には良好な品
質を確保するための品質保証領域が存在するといえる。As described above, in the drawing process of the iridium wire, there is a temperature range in which the wire can be processed in accordance with the processing rate, and this temperature range fluctuates. On the other hand, the machinable region merely indicates whether or not machining can be performed without causing breakage, and does not indicate a range in which a high-quality wire rod having no defect can be machined. That is, it is considered that at a processing temperature near the lower limit value, there is a region in which microcracks occur although no fracture occurs due to the relationship between processing resistance and material strength.
Further, at the processing temperature near the upper limit value, the above-mentioned recrystallization appears not only inside the material but also on the surface, which causes the material surface to become rough. Therefore, regarding the upper limit of the processing temperature, it is necessary to consider the recrystallization temperature which changes due to the change of the processing rate. Therefore, it can be said that there is a quality assurance area for ensuring good quality in the machinable area.
【００１４】これら加工可能温度、欠陥発生温度により
導き出される品質保証領域を図示すると図３のようにな
る。本発明者等は、この品質保証領域内の条件で加工す
ることにより欠陥のない線材を製造できるものとして、
鋭意検討しこの品質保証領域の境界線を明確とすること
とした。FIG. 3 shows the quality assurance region derived from the workable temperature and the defect generation temperature. The inventors of the present invention assume that a wire rod having no defects can be manufactured by processing under the conditions within this quality assurance region.
After careful investigation, we decided to clarify the boundary line of this quality assurance area.
【００１５】即ち、本願に係る引抜き加工方法は、ダイ
ス１パスでの加工率をＸ（％）、ダイス入口での線材加
熱温度をＴ（℃）としたとき、下記式で囲まれる領域内
の加工率、加熱温度で加工することを特徴とするもので
ある。That is, in the drawing method according to the present application, when the processing rate in one pass of the die is X (%) and the heating temperature of the wire rod at the die inlet is T (° C.), It is characterized by processing at a processing rate and a heating temperature.
【００１６】[0016]
【数４】 [Equation 4]
【数５】 [Equation 5]
【数６】 [Equation 6]
【００１７】本発明の数４〜数６により定められる品質
保証領域を図４に示す。この図４では、上述した加工可
能温度上限が数４に、表面荒れ発生温度線が数５に、そ
して、割れ発生温度線が数６に対応する。尚、加工可能
温度下限線は、数４と数６との交点より低い断面減少率
で交錯しないことが本発明者等の検討から明らかとなっ
ているので、加工可能温度下限線は品質保証領域を規定
することはない。また、本発明者によれば、従来のバー
ナー加熱による加工における条件は図４のａ点近傍の温
度、加工率で示され、本発明の品質保証領域の範囲外に
ある。FIG. 4 shows the quality assurance area defined by the equations 4 to 6 of the present invention. In FIG. 4, the upper limit of the processable temperature corresponds to the equation 4, the surface roughness occurrence temperature line corresponds to the equation 5, and the crack occurrence temperature line corresponds to the equation 6. Since it has been clarified by the present inventors that the lower limit line of processable temperature does not intersect at a cross-section reduction rate lower than the intersection point of the equations 4 and 6, the lower limit line of processable temperature is the quality assurance region. Is not specified. According to the inventor of the present invention, the conventional conditions for processing by burner heating are indicated by the temperature and the processing rate in the vicinity of point a in FIG.
【００１８】本発明によれば、加工温度を加工率との関
連から適正な範囲とすることで、高品質の線材の引抜き
加工が可能となる。また、本発明によれば最大限の加工
率（数４及び数６の交差点であり約３０％である）での
加工を行なうことができ、１回の加工による断面減少効
果に優れ効率的な加工が可能である。これは、上述のよ
うに所望の線径の線材を製造するためには引抜き加工を
複数回繰り返し加工することとなるが、本発明によれ
ば、１回当たりの加工率を最大限に設定することでその
加工パス数を最小とすることが可能となる。According to the present invention, by setting the working temperature in an appropriate range in relation to the working rate, it becomes possible to carry out drawing work of a high-quality wire rod. Further, according to the present invention, it is possible to perform the processing at the maximum processing rate (the intersection of the equations 4 and 6 and is about 30%), which is excellent in the cross-sectional reduction effect by one-time machining and is efficient. It can be processed. As described above, in order to manufacture a wire rod having a desired wire diameter as described above, the drawing process is repeated a plurality of times, but according to the present invention, the processing rate per time is set to the maximum. As a result, the number of processing passes can be minimized.
【００１９】また、本発明に係る加工方法における線材
の加熱温度は従来のものより低くなることから、線材と
接触するダイスに与えるダメージを低減することができ
ダイスの寿命の長期化を図ることができる。Further, since the heating temperature of the wire in the processing method according to the present invention is lower than that of the conventional one, damage to the die contacting the wire can be reduced and the life of the die can be extended. it can.
【００２０】ところで、複数回繰り返し加工を行ない細
径の線材を製造する際には、加工する材料によっては各
加工パス間で中間焼鈍を行なう必要がある場合がある。
これは、引抜き加工を数回繰り返すことで加工硬化が進
展し、材料割れを生じることがあることから、数パス加
工後に中間焼鈍することで材料に回復現象を生じさせ再
び加工可能な状態にするものである。そして、この中間
焼鈍は引抜き加工時の加熱温度が低い程、頻繁に行う必
要が生じてくるが、中間焼鈍工程を頻繁に行うことは全
体の加工時間を増大させることとなる。そこで、本願発
明における加工温度のうちより好ましい範囲としては、
Ｔ＝７５０の線より上の領域、即ち、７５０℃以上で再
結晶が生じない温度範囲とするのが好ましい。かかる範
囲とすることで中間焼鈍の実施回数を極力減らすことが
できるからである。尚、この中間焼鈍の要否及び焼鈍温
度は、合金種により加工硬化挙動ならびに回復挙動が異
なることから、合金種により異なる。例えば、イリジウ
ム−白金合金では１０００℃〜１１００℃の中間焼鈍が
必要であり、イリジウム−ロジウム合金においても場合
によっては９００℃〜１０００℃の中間焼鈍が必要とな
ることがある。By the way, when a wire having a small diameter is manufactured by repeating the working a plurality of times, it may be necessary to perform intermediate annealing between the working passes depending on the material to be worked.
This is because work hardening sometimes progresses by repeating drawing several times and material cracks may occur, so by intermediate annealing after several passes of processing, a recovery phenomenon occurs in the material and it becomes possible to work again. It is a thing. The intermediate annealing needs to be performed more frequently as the heating temperature at the time of drawing is lower. However, frequent execution of the intermediate annealing process increases the total processing time. Therefore, as a more preferable range of the processing temperature in the present invention,
It is preferable to set the region above the line of T = 750, that is, the temperature range in which recrystallization does not occur at 750 ° C. or higher. This is because the number of times the intermediate annealing is performed can be reduced as much as possible by setting such a range. The necessity of this intermediate annealing and the annealing temperature differ depending on the alloy type because the work hardening behavior and the recovery behavior differ depending on the alloy type. For example, the iridium-platinum alloy requires intermediate annealing at 1000 ° C to 1100 ° C, and the iridium-rhodium alloy may also require intermediate annealing at 900 ° C to 1000 ° C depending on the case.
【００２１】尚、本発明における加工速度（引き抜き速
度）については、特に限定されるものではない。例え
ば、従来のバーナー加熱による加工の加工速度は０.５
〜１.０ｍ／ｍｉｎであるが、本発明でもこの速度での
加工が可能であるが、加工条件を適正化していることか
ら、従来の加工速度より高速での加工も可能である。そ
して、好ましい加工速度は１.０〜３.０ｍ／ｍｉｎであ
る。The processing speed (drawing speed) in the present invention is not particularly limited. For example, the processing speed for conventional burner heating is 0.5
Although it is ~ 1.0 m / min, it is possible to process at this speed in the present invention as well, but since the processing conditions are optimized, processing at a higher speed than the conventional processing speed is also possible. And the preferable processing speed is 1.0 to 3.0 m / min.
【００２２】一方、本発明は引抜き加工時の温度を従来
よりも低くし、更にその下限値の好ましいものを約７５
０℃とすることから、比較的狭い温度範囲で加工するこ
とを特徴とするものである。従って、本発明において
は、加工温度の制御を適正に行なうことが重要となる。
一方、従来の引抜き加工で行われているバーナーの火炎
では加工温度が高くなりすぎ、本発明で目的とする温度
域での制御は困難である。そこで、本発明者等は加熱温
度を従来より低く設定することができ、且つその制御が
容易な手法として通電加熱法、即ち、被加工材である線
材に電流を流すことにより線材を加熱し加工するのが好
ましいとする。On the other hand, according to the present invention, the temperature at the time of drawing is set lower than before, and the lower limit is preferably about 75.
Since it is set to 0 ° C., it is characterized in that it is processed in a relatively narrow temperature range. Therefore, in the present invention, it is important to properly control the processing temperature.
On the other hand, with the flame of the burner used in the conventional drawing process, the processing temperature becomes too high, and it is difficult to control in the temperature range targeted by the present invention. Therefore, the inventors of the present invention can set the heating temperature lower than the conventional one, and as a method of easily controlling the heating temperature, that is, an electric heating method, that is, heating the wire rod by passing an electric current through the wire rod to be processed. It is preferable to do this.
【００２３】この加熱方法は線材に電流を流すことで発
生する抵抗熱を加工のための熱源とするものであるが、
このときの線材温度は印加する電流を調整することで設
定することができる。従って、この通電加熱法によれ
ば、従来のバーナー加熱に比べて加工温度を低めに設定
することができ更に安定させることができる。そして、
これにより加工条件を適切な範囲で維持することができ
るため、高品質の線材を効率的に製造することができ
る。This heating method uses resistance heat generated by passing an electric current through the wire as a heat source for processing.
The wire temperature at this time can be set by adjusting the applied current. Therefore, according to this energization heating method, the processing temperature can be set lower than that of the conventional burner heating and can be further stabilized. And
As a result, the processing conditions can be maintained in an appropriate range, so that a high quality wire rod can be efficiently manufactured.
【００２４】この線材の通電加熱は、具体的には、一対
の電極を線材に接触させて通電することによりなされる
が、線材がダイスを通過する前に所定温度になるよう通
電する必要がある。この場合、双方の電極をダイス入口
側に設置しこれらを線材に接触させて通電しても良い
が、好ましいのは、一方の電極をダイスの入口側に離隔
設置し他方の電極はダイスの出口側で且つダイスに近接
させるのものである。双方の電極をダイス入口側に配し
た場合、線材の加熱がダイスに導入される前に終了して
しまい、加工途中に温度低下が生じ予定されていた加工
条件での加工ができないからである。また、他方の電極
をダイスの出口側で且つダイスに近接させるのは他方の
電極をダイスから離して設置すると加工終了後も線材が
加熱されるため線材の破断が生じることがあるからであ
る。ここでの出口側電極とダイス出口面との間隔は１０
０ｍｍ以下とするのが好ましい。但し、最も効率的に線
材を通電するためには、このダイス出口側の電極をダイ
スに接触させた状態で配置して電流がダイスを通過する
状態とし、電極及びダイスの双方により線材を通電する
ようにするのが特に好ましいものである。The heating of the wire by energization is specifically carried out by bringing a pair of electrodes into contact with the wire to energize it, but it is necessary to energize the wire to a predetermined temperature before passing through the die. . In this case, both electrodes may be installed on the die inlet side and they may be brought into contact with the wire to energize, but it is preferable that one electrode is installed separately on the die inlet side and the other electrode is the die outlet. It is on the side and close to the dice. This is because, when both electrodes are arranged on the die inlet side, the heating of the wire is terminated before being introduced into the die, and the temperature cannot be reduced during the machining, and the machining cannot be performed under the machining conditions that are planned. Further, the reason why the other electrode is placed on the exit side of the die and close to the die is that if the other electrode is installed away from the die, the wire may be heated even after the processing is finished and the wire may break. The distance between the exit side electrode and the die exit surface is 10
It is preferably 0 mm or less. However, in order to energize the wire most efficiently, the electrode on the die exit side is placed in contact with the die so that the current passes through the die, and the wire is energized by both the electrode and the die. It is particularly preferable to do so.
【００２５】一方、ダイス入口側に離隔設置する電極の
位置は、ダイスから４５０〜５５０ｍｍ上流側とするの
が好ましい。後述するように、この引き抜き加工では線
材に潤滑剤を塗布するのが好ましいが、この電極の設置
位置をあまりにダイスに近くすると、線材温度が直ちに
上昇し塗布した潤滑剤が沸騰してしまい，均一に塗布す
ることができなくなるからであり、また、塗布作業のた
めのスペースが確保できなくなるからである。更に、温
度測定のスペース確保ならびに線材温度コントロールを
なるべく容易にするため電極の設置間隔がある程度必要
となるからである。尚、このダイス入口側に離隔配置さ
れる電極の材質は、カーボンを用いるのが好ましい。On the other hand, the position of the electrode spaced apart from the die entrance side is preferably 450 to 550 mm upstream from the die. As will be described later, it is preferable to apply a lubricant to the wire in this drawing process, but if the installation position of this electrode is too close to the die, the wire temperature will rise immediately and the applied lubricant will boil, resulting in a uniform This is because it is no longer possible to apply the coating solution to the coating solution and the space for the coating operation cannot be secured. Furthermore, it is necessary to provide a certain interval between the electrodes in order to secure a space for temperature measurement and control the wire temperature as easily as possible. It is preferable that carbon is used as the material of the electrodes spaced apart from the die entrance side.
【００２６】そして、本発明に係る引抜き加工方法にお
いては、線材の加熱に加えて、ダイスも加熱して加工を
行うことがより好ましい。ダイスを加熱することにより
加工途中の線材の温度低下を抑制することができるた
め、これにより線材の破断を確実に防止することができ
るからである。このダイスの加熱温度としては、４００
〜７００℃の範囲とするのが好ましく、ダイス外周に電
気ヒーターを設置しこれにより行なうことができる。In the drawing method according to the present invention, it is more preferable that the die is also heated in addition to the heating of the wire. By heating the die, it is possible to suppress the temperature drop of the wire rod during processing, and thus it is possible to reliably prevent the wire rod from breaking. The heating temperature of this die is 400
The temperature is preferably in the range of ˜700 ° C., and this can be performed by installing an electric heater around the die.
【００２７】更に、この引き抜き加工においては、加工
後の線材の品質の確保、加工効率の確保のために、線材
に潤滑剤を塗布した後加工するのが好ましい。この潤滑
剤としては、主成分がカーボンであるカーボン系潤滑材
を適用するのが好ましい。カーボン潤滑剤は本発明にお
ける温度下において劈開し微細に粉砕することで滑らか
となり、線材に傷を発生させることなく加工を補助でき
るからである。この点、カーボン系潤滑剤は、大気中で
ＣＯならびにＣＯ２へと酸化されることにより消費され
てしまい、従来の引き抜き加工における加工温度（１３
００℃）ではその酸化速度が非常に速く使用が困難であ
る。そのため従来法では、上述のように窒化ホウ素系の
潤滑剤を適用しているが、窒化ホウ素系の潤滑剤は揮発
はしないものの硬く、劈開することなく線材を傷つける
ことがある。従って、本発明はカーボン系潤滑剤の使用
を可能としたことにより傷の発生しない高品質の線材を
製造することができるというメリットもある。Further, in this drawing work, it is preferable to apply a lubricant to the wire material and then work it in order to ensure the quality of the wire material after processing and the processing efficiency. As this lubricant, it is preferable to apply a carbon-based lubricant whose main component is carbon. This is because the carbon lubricant becomes smooth by being cleaved and finely pulverized at the temperature in the present invention, and the processing can be assisted without causing scratches on the wire. In this respect, the carbon-based lubricant is consumed by being oxidized into CO and CO 2 in the atmosphere, and the processing temperature (13
At 00 ° C., the oxidation rate is very high and it is difficult to use. Therefore, in the conventional method, the boron nitride-based lubricant is applied as described above. However, although the boron nitride-based lubricant does not volatilize, it is hard and may damage the wire without cleaving. Therefore, the present invention has an advantage that it is possible to manufacture a high-quality wire material which does not cause scratches because the carbon-based lubricant can be used.
【００２８】また、本発明により実現されるカーボン系
潤滑剤の適用により、線材の品質向上と共にダイス寿命
のさらなる向上というメリットもある。従来法で使用さ
れている窒化ホウ素系潤滑剤は、セラミックスの１種で
ありダイスに対して研磨作用があるが、カーボン系潤滑
剤にはかかる研磨作用はないからである・Further, by applying the carbon-based lubricant realized by the present invention, there is an advantage that the quality of the wire is improved and the die life is further improved. This is because the boron nitride-based lubricant used in the conventional method is a type of ceramic and has a polishing action on the die, but the carbon-based lubricant does not have such a polishing action.
【００２９】[0029]
【発明の実施の形態】以下に本発明の好適な実施形態を
図面と共に示す。BEST MODE FOR CARRYING OUT THE INVENTION Preferred embodiments of the present invention will be described below with reference to the drawings.
【００３０】第１実施形態：本実施形態では、イリジウ
ム合金としてイリジウム−白金合金（Ｉｒ−５％Ｐｔ）
よりなる線材を製造した。イリジウム２０９ｇと白金１
１ｇとを秤量、混合し、これをＡｒアーク炉にて溶解
し、イリジウム合金インゴットを製造した。そして、こ
のイリジウム合金インゴットを１５００℃で熱間鍛造し
た。加工後のインゴットの寸法は１０ｍｍ角、長さ９０
ｍｍとした。次にこの角材を１３００℃に加熱した溝付
ロールに通過させることにより熱間圧延して断面径を更
に減少させた後、大気雰囲気で１４００℃、３０分焼鈍
した後、熱間スエージングを行った。スエージング加工
は、鍛造機としてロータリースエージャーを用い、加工
温度を１３００℃とし、加圧周期５０Ｈｚとした。この
スエージング加工による総合加工率は７５％で、加工後
のイリジウム合金線材は直径３.１０ｍｍの断面円形の
ものとなった First Embodiment : In this embodiment, an iridium-platinum alloy (Ir-5% Pt) is used as the iridium alloy.
Was manufactured. Iridium 209g and platinum 1
1 g was weighed and mixed, and this was melted in an Ar arc furnace to produce an iridium alloy ingot. Then, this iridium alloy ingot was hot forged at 1500 ° C. The size of the ingot after processing is 10mm square and length 90
mm. Next, this square bar is hot-rolled by passing it through a grooved roll heated to 1300 ° C. to further reduce the cross-sectional diameter, and then annealed at 1400 ° C. for 30 minutes in an air atmosphere, followed by hot swaging. It was In the swaging process, a rotary swager was used as a forging machine, the processing temperature was 1300 ° C., and the press cycle was 50 Hz. The total processing rate by this swaging is 75%, and the processed iridium alloy wire has a circular cross section with a diameter of 3.10 mm.
【００３１】そして、熱間スエージング加工後のイリジ
ウム合金線材を引抜き加工により細線とした。引抜き加
工は、図５で示すような方法にて行なった。図５におい
て被加工材である線材１は、ダイス上流側のロール電極
２とダイス３の出口側の電極を兼ねるダイス保持板４と
により通電加熱されダイス３を通過することで加工され
る。線材温度は赤外線放射温度計により測定されその値
をもとにプログラム式コントローラー５で線材に印加す
る電気量を調節している。また、通電ロール２を通過し
た線材には潤滑剤６を塗布した後にダイスに送り込む。
ダイス３は電気ヒーター７により６５０℃に加熱されて
いる。尚、本実施形態では、ダイスと通電ロールとの間
隔を５２０ｍｍとし、加熱温度は１０００℃となるよう
通電量を制御している。The iridium alloy wire rod after the hot swaging process was drawn into a fine wire. The drawing process was performed by the method as shown in FIG. In FIG. 5, the wire material 1 as a material to be processed is electrically heated by the roll electrode 2 on the upstream side of the die and the die holding plate 4 also serving as the electrode on the outlet side of the die 3, and is processed by passing through the die 3. The wire temperature is measured by an infrared radiation thermometer, and the amount of electricity applied to the wire is adjusted by the program controller 5 based on the value. Further, the wire 6 that has passed through the energizing roll 2 is coated with a lubricant 6 and then fed into a die.
The die 3 is heated to 650 ° C. by the electric heater 7. In this embodiment, the distance between the die and the energizing roll is 520 mm, and the energizing amount is controlled so that the heating temperature is 1000 ° C.
【００３２】そして、この装置により、ダイス１パスに
おける平均断面減少率１７.５％とし、伸線速度を１.０
〜２.３ｍ／ｍｉｎ間に設定してダイス孔径を順次減少
させて合金線材を繰り返し引抜き加工し、最終的に径
０．６ｍｍの細線とした。尚、この繰り返し引抜き工程
を行なうに当たっては、２〜４パス毎に中間焼鈍（１１
００℃、３０ｍｉｎ）を行なっている。With this apparatus, the average area reduction rate in one pass of the die was set to 17.5%, and the wire drawing speed was set to 1.0.
The diameter of the die hole was gradually reduced by setting the speed to ˜2.3 m / min, and the alloy wire rod was repeatedly drawn to finally obtain a fine wire having a diameter of 0.6 mm. In performing the repeated drawing step, the intermediate annealing (11
00 ° C., 30 min).
【００３３】そして、この製造したイリジウム−白金合
金線材につき、材料組織及び欠陥の有無を検査したとこ
ろ、材料組織はほぼ均一であり、微小なものも含め欠陥
がないことが確認された。Then, the manufactured iridium-platinum alloy wire was inspected for material structure and presence or absence of defects, and it was confirmed that the material structure was almost uniform and there were no defects including minute ones.
【００３４】比較例：第１実施形態に対する比較とし
て、従来の方法によりイリジウム−白金合金線材を製造
した。従来法によるイリジウム合金線材の製造は、図６
の製造装置により行なっており、バーナー８としてプロ
パン燃焼バーナーを用いた。また、潤滑剤は窒化ホウ素
系潤滑剤を塗布している。 Comparative Example : As a comparison with the first embodiment, an iridium-platinum alloy wire rod was manufactured by a conventional method. The iridium alloy wire produced by the conventional method is shown in FIG.
The propane combustion burner was used as the burner 8. As the lubricant, a boron nitride lubricant is applied.
【００３５】そして、第１実施形態と同様の圧延、スエ
ージングにより製造したイリジウム合金線材について、
ダイス１パス当たりの平均断面減少率９.７％とし、伸
線速度を０.５〜０.７ｍ／ｍｉｎ間で設定して複数回繰
り返し引抜き加工した。尚、この比較例における加工
率、伸線速度は第１実施形態のものより低く設定した
が、これはバーナー加熱による加工温度（約１３００
℃）が高すぎるために、第１実施形態と同じ加工率等で
加工を行なうと、線材表面に荒れ、皺が発生すると共に
線材破断が発生し易いことからこれより低い値としたも
のである。また、このバーナー加熱による引抜き加工で
は、加工温度が１３００℃と高いことから中間焼鈍を行
なう必要はないため、行なっていない。Then, with respect to the iridium alloy wire rod manufactured by rolling and swaging similar to the first embodiment,
The average cross-section reduction rate per one pass of the die was set to 9.7%, and the drawing speed was set to 0.5 to 0.7 m / min. The working ratio and the wire drawing speed in this comparative example were set lower than those in the first embodiment, but this was set at the working temperature (about 1300) by the burner heating.
(° C.) Is too high, so that when the processing is performed at the same processing rate as in the first embodiment, the surface of the wire is roughened, wrinkles are easily generated, and the wire is easily broken. . Further, in the drawing work by the burner heating, since the working temperature is as high as 1300 ° C., it is not necessary to carry out the intermediate annealing, so that it is not carried out.
【００３６】この比較例における引抜き工程でも製造さ
れた線材に破断や大きな欠陥はなかったが、この比較例
においては、線材表面に荒れ，皺が生じ、これを除去す
るために加工途中で線材表面を研磨しなければならなか
った。また、比較例は加工温度が高温であり、そのため
に使用した窒化ホウ素系潤滑材の粒子が劈開しないため
に線材表面に潤滑剤粒子によるスクラッチが観察され
た。Although the wire rod produced in the drawing step in this comparative example did not have fractures or large defects, in this comparative example, the surface of the wire rod was roughened or wrinkled, and in order to remove it, the surface of the wire rod was removed during processing. Had to be polished. In the comparative example, the processing temperature was high, and the particles of the boron nitride-based lubricant used therefor did not cleave, so that scratches due to the lubricant particles were observed on the surface of the wire.
【００３７】また、破断が生じないとはいっても、これ
は破断が生じないように加工条件を制限したことによる
ものである。そして、このように制限された加工条件下
では同じ径の線材を製造するためのパス数（加工数）が
第１実施形態よりも大きくなり、第１実施形態では１.
８８倍のパス回数が必要となった。また、全加工時間も
比較例は大きく、第１実施形態では中間焼鈍の時間を考
慮しても比較例は中間焼鈍がないにもかかわらず１.７
６倍の時間を要した。従って、第１実施形態の引抜き加
工方法は高品質の線材をより短いパス数、時間で製造可
能であることが確認できる。Further, although the fracture does not occur, this is because the processing conditions are restricted so that the fracture does not occur. Then, the number of passes (the number of passes) for producing the wire having the same diameter is larger than that in the first embodiment under the processing conditions thus limited, and in the first embodiment, 1.
88 times more passes were needed. Further, the total working time is also large in the comparative example, and even if the time for the intermediate annealing is taken into consideration in the first embodiment, the comparative example is 1.7 even though there is no intermediate annealing.
It took six times as long. Therefore, it can be confirmed that the drawing method of the first embodiment can manufacture a high-quality wire rod in a shorter number of passes and in a shorter time.
【００３８】第２実施形態：本実施形態では、イリジウ
ム合金としてイリジウム−ロジウム合金（Ｉｒ−２０％
Ｒｈ）よりなる線材を製造した。イリジウム１６０ｇと
ロジウム４０ｇとを秤量、混合し、これをＡｒアーク炉
にて溶解し、イリジウム合金インゴットを製造した。 Second Embodiment : In this embodiment, an iridium-rhodium alloy (Ir-20%) is used as the iridium alloy.
A wire consisting of Rh) was produced. 160 g of iridium and 40 g of rhodium were weighed and mixed, and this was melted in an Ar arc furnace to manufacture an iridium alloy ingot.
【００３９】このイリジウム合金インゴットを第１実施
形態と同様に、熱間鍛造、熱間スェージングを行なっ
た。ここでの加工条件は、鍛造温度は１５００℃とし、
熱間スェージングは、加工温度を１３００℃とし、加圧
周期５０Ｈｚとした。そして、スエージング加工により
直径３.１０ｍｍの断面円形のイリジウム合金線材とし
た。This iridium alloy ingot was subjected to hot forging and hot swaging as in the first embodiment. The processing conditions here are that the forging temperature is 1500 ° C.,
The hot swaging was performed at a processing temperature of 1300 ° C. and a pressure cycle of 50 Hz. Then, an iridium alloy wire rod having a circular cross section with a diameter of 3.10 mm was obtained by swaging.
【００４０】そして、第１実施形態と同様、通電加熱に
よりダイス１パスの平均断面減少率１７.５％，伸線速
度１.０〜２.３ｍ／ｍｉｎ間で設定し引抜き加工を行な
った。 尚、白金―ロジウム合金の場合、中間焼鈍を行
なう必要がないので行なっていない。Then, similarly to the first embodiment, the drawing was carried out by setting the average cross-section reduction rate of 1 pass of the die to 17.5% and the wire drawing speed of 1.0 to 2.3 m / min by the electric heating. Incidentally, in the case of a platinum-rhodium alloy, it is not necessary to perform intermediate annealing, so it is not performed.
【００４１】この結果製造された線材は第１実施系他と
同様良好な品質のものであり、ほぼ均一な材料組織であ
り、欠陥がないことが確認された。尚、このイリジウム
―ロジウム合金についても、比較例１のように従来法で
あるバーナー加熱による引抜き加工を行なったが、この
場合の加工パス数は第２実施形態の２.０倍であった。
そして、全加工時間も第２実施形態の３.７６倍であっ
た。従って、イリジウム―ロジウム合金線材の製造にあ
たっても本発明は効率に優れた加工方法であることがわ
かった。As a result, it was confirmed that the produced wire had a good quality as in the first embodiment and the like, had a substantially uniform material structure, and had no defects. Note that this iridium-rhodium alloy was also subjected to the conventional drawing method by burner heating as in Comparative Example 1, but the number of processing passes in this case was 2.0 times that of the second embodiment.
The total processing time was 3.76 times longer than that in the second embodiment. Therefore, it was found that the present invention is a highly efficient processing method even when manufacturing an iridium-rhodium alloy wire.
【００４２】[0042]
【発明の効果】以上説明したように本発明によれば、割
れや組織的不均一等の欠陥を有しない極めて優れた品質
のイリジウム又はイリジウム合金線材を効率的に製造す
ることができる。そのため、本発明により製造されるイ
リジウム又はイリジウム合金線材は、点火プラグ用電極
等のような今後の需要の拡大が予測され、品質基準の厳
格な機能材料としての用途への適用が期待できる。As described above, according to the present invention, it is possible to efficiently manufacture an iridium or iridium alloy wire rod of extremely excellent quality that does not have defects such as cracks and structural nonuniformity. Therefore, the demand for the iridium or iridium alloy wire rod manufactured by the present invention is expected to increase in the future, such as electrodes for spark plugs, and it can be expected to be applied to applications as functional materials with strict quality standards.
【図１】イリジウム合金線材の常温及び高温での引き抜
き加工時の破断状況を示す図。FIG. 1 is a diagram showing a fracture state of an iridium alloy wire rod during drawing at normal temperature and high temperature.
【図２】イリジウム合金線材を引き抜き加工する際の加
工可能領域を示す図。FIG. 2 is a diagram showing a workable region when an iridium alloy wire rod is drawn.
【図３】イリジウム合金線材を引き抜き加工する際の品
質保証領域を示す図。FIG. 3 is a diagram showing a quality assurance region when an iridium alloy wire rod is drawn.
【図４】本発明に係る引き抜き加工条件を詳細に示す
図。FIG. 4 is a diagram showing details of drawing processing conditions according to the present invention.
【図５】第１及び第実施形態の通電加熱法によるイリジ
ウム合金の引き抜き加工工程を示す図。FIG. 5 is a diagram showing a drawing process of the iridium alloy by the electric heating method of the first and the first embodiments.
【図６】従来のバーナー加熱によるイリジウム合金の引
き抜き加工工程を示す図。FIG. 6 is a diagram showing a conventional iridium alloy drawing process by burner heating.
１ イリジウム合金線材 ２ ロール電極 ３ ダイス ４ ダイス保持板 ５ プログラム式コントローラー ６ 潤滑剤 ７ 電気ヒーター ８ バーナー ９ 火炎 1 Iridium alloy wire 2 roll electrode 3 dice 4 Die holding plate 5 Programmable controller 6 lubricant 7 Electric heater 8 burners 9 flames
フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｃ２１Ｄ 1/10 Ｃ２１Ｄ 1/10 Ａ (72)発明者 武石 誠司 神奈川県伊勢原市鈴川26番地 田中貴金属 工業株式会社伊勢原工場内 (72)発明者 中山 覚史 神奈川県伊勢原市鈴川26番地 田中貴金属 工業株式会社伊勢原工場内 (72)発明者 人見 聡一 神奈川県伊勢原市鈴川26番地 田中貴金属 工業株式会社伊勢原工場内 Ｆターム(参考） 4E096 EA08 EA12 FA01 HA22 JA01 JA13 KA01 KA04 KA05 Continuation of front page (51) Int.Cl. 7 Identification code FI theme code (reference) C21D 1/10 C21D 1/10 A (72) Inventor Seiji Takeishi 26 Suzukawa, Isehara City, Kanagawa Prefecture Tanaka Kikinzoku Kogyo Co., Ltd. Isehara Factory (72) Inventor Satoshi Nakayama 26 Suzukawa, Isehara City, Kanagawa Prefecture, Tanaka Kikinzoku Kogyo Co., Ltd., Isehara Plant (72) Inventor, Soichi 26 Suzukawa, Isehara City, Kanagawa Prefecture, F Term, Isehara Plant, Tanaka Kikinzoku Kogyo Co., Ltd. Reference) 4E096 EA08 EA12 FA01 HA22 JA01 JA13 KA01 KA04 KA05
Claims (10)
材を加熱してダイスに通過させて引抜き加工する方法に
おいて、 ダイス1パスでの加工率をＸ（％）、ダイス入口での線
材加熱温度をＴ（℃）としたとき、下記式で囲まれる領
域内の加工率、加熱温度で加工することを特徴とするイ
リジウム又はイリジウム合金線材の引抜き加工方法。 【数１】 【数２】 【数３】 1. A method of heating a wire made of iridium or an iridium alloy and passing it through a die to perform a drawing process, wherein the processing rate in one pass of the die is X (%), and the heating temperature of the wire at the die inlet is T ( [Deg.] C.), a method of drawing an iridium or iridium alloy wire rod, which comprises working at a working rate in a region surrounded by the following formula and a heating temperature. [Equation 1] [Equation 2] [Equation 3]
１記載のイリジウム又はイリジウム合金線材の引抜き加
工方法。2. The method for drawing an iridium or iridium alloy wire rod according to claim 1, further comprising working at T = 750 ° C. or higher.
ダイスから離隔配置し、他方の電極をダイス出口側にダ
イスに近接配置し、前記一対の電極を線材に接触させて
通電する請求項１又は請求項２記載のイリジウム又はイ
リジウム合金線材の引抜き加工方法。3. One of the pair of electrodes is disposed on the die inlet side away from the die, and the other electrode is disposed on the die outlet side in proximity to the die, and the pair of electrodes are brought into contact with a wire to conduct electricity. A method for drawing iridium or an iridium alloy wire according to claim 1 or 2.
状態で配置することにより電流を該ダイスに通過させ、
該電極及び該ダイスにより線材を通電する請求項３記載
のイリジウム又はイリジウム合金線材の引抜き加工方
法。4. A current is passed through the die by arranging the electrode on the die exit side in contact with the die,
The method of drawing an iridium or iridium alloy wire according to claim 3, wherein the wire is energized by the electrode and the die.
がカーボンである請求項１〜請求項４記載のイリジウム
又はイリジウム合金線材の引抜き加工方法。5. The iridium or iridium alloy wire rod drawing method according to claim 1, wherein the material of the electrodes spaced apart from the die inlet side is carbon.
項５記載のイリジウム又はイリジウム合金線材の引抜き
加工方法。6. The method for drawing an iridium or iridium alloy wire rod according to claim 1, wherein the die is heated and processed.
ヒーターによりダイスを加熱する請求項６記載のイリジ
ウム又はイリジウム合金線材の引抜き加工方法。7. The method of drawing an iridium or iridium alloy wire according to claim 6, wherein an electric heater is installed on the outer periphery of the die and the die is heated by the electric heater.
行なう請求項６又は請求項７記載のイリジウム又はイリ
ジウム合金線材の引抜き加工方法。8. The method for drawing an iridium or iridium alloy wire rod according to claim 6 or 7, which is performed by heating the die temperature to 400 to 700 ° C.
る請求項１〜請求項８記載のイリジウム又はイリジウム
合金線材の引抜き加工方法。9. The method for drawing iridium or an iridium alloy wire according to claim 1, wherein the method is carried out after applying a lubricant between the pair of electrodes.
する請求項９記載のイリジウム又はイリジウム合金線材
の引抜き加工方法。10. The method for drawing an iridium or iridium alloy wire rod according to claim 9, wherein a lubricant whose main component is carbon is applied.
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| JP2001251241A JP3647029B2 (en) | 2001-08-22 | 2001-08-22 | Drawing method of iridium or iridium alloy wire |
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| JP2001251241A JP3647029B2 (en) | 2001-08-22 | 2001-08-22 | Drawing method of iridium or iridium alloy wire |
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