JP5098753B2 - Manufacturing method of ultra-high purity aluminum high rolled material - Google Patents
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本発明は、超高純度アルミニウム高圧延材の製造方法に関し、詳しくは純度９９．９９９９％以上の超高純度アルミニウム鋳塊材に熱間圧延処理を施して熱間圧延材を得、この熱間圧延材に冷間圧延処理を施すことにより、加工率４０％超で、十分な硬度の高圧延材を製造する方法に関する。 The present invention relates to a method for producing ultra-high purity aluminum high-rolled material, and more specifically, a hot-rolled material is obtained by subjecting an ultra-high-purity aluminum ingot material having a purity of 99.9999% or more to hot rolling. The present invention relates to a method for producing a high-rolled material with sufficient hardness at a processing rate exceeding 40% by subjecting the rolled material to a cold rolling process.
純度９９．９９％未満の普通アルミニウム鋳塊材から圧延材を製造する方法としては、この鋳塊材に熱間圧延処理を施して熱間圧延材を得、この熱間圧延材に冷間圧延処理を施す方法が広く用いられている。〔特許文献１：特開平８−３０２４５０号公報〕。 As a method of producing a rolled material from a normal aluminum ingot having a purity of less than 99.99%, a hot rolled material is obtained by subjecting the ingot material to a hot rolling process, and the hot rolled material is cold-rolled. A method of performing processing is widely used. [Patent Document 1: JP-A-8-302450].
しかし、かかる従来の製造方法を純度９９．９９９９％以上の超高純度アルミニウム鋳塊材に適用して、この熱間圧延材に対する加工率が４０％超の高圧延材を得ようとすると、その硬度が不十分なものとなり易いことが分かった。硬度が不十分な高圧延材は、これに冷間圧延処理、矯正処理、洗浄処理などを施すと、表面の平滑度が低くなり、また極低温での電気伝導度、熱伝導度が不十分なものとなる。 However, when such a conventional manufacturing method is applied to an ultra-high purity aluminum ingot material having a purity of 99.9999% or more and an attempt is made to obtain a high-rolled material having a processing rate of more than 40% for this hot-rolled material, It was found that the hardness tends to be insufficient. High-rolled material with insufficient hardness, when subjected to cold rolling treatment, straightening treatment, cleaning treatment, etc., the surface smoothness becomes low, and electrical conductivity and thermal conductivity at extremely low temperatures are insufficient. It will be something.
そこで本発明者は、純度９９．９９９９％以上の超高純度アルミニウム鋳塊材に熱間圧延処理を施して熱間圧延材を得、この熱間圧延材に冷間圧延処理を施すことにより、加工率４０％超で、十分な硬度の高圧延材を製造しうる方法を開発するべく鋭意検討した結果、本発明に至った。 Therefore, the present inventor performs a hot rolling treatment on an ultra-high purity aluminum ingot material having a purity of 99.9999% or more to obtain a hot rolling material, and by subjecting the hot rolling material to a cold rolling treatment, As a result of intensive studies to develop a method capable of producing a high-rolled material with sufficient hardness at a processing rate exceeding 40%, the present invention has been achieved.
すなわち本発明は、純度９９．９９９９％以上の超高純度アルミニウム鋳塊材に加工温度２６０℃以上の熱間圧延処理を施すことにより熱間圧延材を得、
得られた熱間圧延材に圧延処理を施して、該熱間圧延材に対する加工率が４０％超の超高純度アルミニウム高圧延材を製造する方法であり、
前記熱間圧延材に、１パス加工率３０％超４０％未満で加工温度１１０℃以上２６０℃未満の冷間圧延処理を３時間以内の処理間隔で繰り返し施すことを特徴とする前記高純度アルミニウム高圧延材の製造方法を提供するものである。
That is, the present invention obtains a hot-rolled material by subjecting an ultra-high purity aluminum ingot material having a purity of 99.9999% or more to a hot rolling process at a processing temperature of 260 ° C. or more,
It is a method of subjecting the obtained hot rolled material to a rolling treatment to produce an ultra-high purity aluminum high rolled material having a processing rate of more than 40% with respect to the hot rolled material,
The high-purity aluminum, wherein the hot-rolled material is repeatedly subjected to a cold rolling process at a processing temperature of 110 ° C. or higher and lower than 260 ° C. at a processing interval of 3 hours or less at a processing rate of more than 30% and less than 40%. A method for producing a highly rolled material is provided.
本発明の製造方法によれば、純度９９．９９９９％以上の超高純度アルミニウム鋳塊材に熱間圧延処理を施して得られた熱間圧延材から、冷間圧延処理により、加工率４０％超で、表面に荒れのない圧延材を製造することができる。 According to the production method of the present invention, a hot rolling material obtained by subjecting an ultra-high purity aluminum ingot material having a purity of 99.9999% or more to hot rolling treatment is subjected to a cold rolling treatment to obtain a processing rate of 40%. A rolled material that is super and has no surface roughness can be produced.
〔超高純度アルミニウム鋳塊材〕
本発明の製造方法に適用される超高純度アルミニウム鋳塊材は、純度９９．９９９９％以上、通常は９９．９９９９９％未満であり、例えば超高純度アルミニウムを加熱溶融して溶湯とし、得られた超高純度アルミニウム溶湯を冷却固化させる通常の方法で得ることができる。溶湯の温度は超高純度アルミニウムの溶融温度以上であり、通常は７００℃〜８００℃である。超高純度アルミニウムの加熱溶融は、通常、真空中あるいは窒素ガス、アルゴンガスなどの不活性ガス雰囲気下に、黒鉛製ルツボ内で行われる。超高純度アルミニウム溶湯の冷却固化は通常、例えば鋳鉄製鋳型内、黒鉛製鋳型内などで行われる。
[Ultra high purity aluminum ingot material]
The ultra-high purity aluminum ingot material applied to the production method of the present invention has a purity of 99.9999% or more, usually less than 99.99999%. For example, ultra high-purity aluminum is heated and melted to obtain a molten metal. In addition, it can be obtained by an ordinary method of cooling and solidifying molten ultrahigh purity aluminum. The temperature of the molten metal is equal to or higher than the melting temperature of ultra high purity aluminum, and is usually 700 ° C to 800 ° C. Ultra high-purity aluminum is usually heated and melted in a graphite crucible in vacuum or in an inert gas atmosphere such as nitrogen gas or argon gas. The cooling and solidification of the ultra-high purity molten aluminum is usually performed, for example, in a cast iron mold or a graphite mold.
超高純度アルミニウム鋳塊材の純度は質量百分率で表わされ、通常、
Ｆｅ、Ｓｉ、Ｃｕ、Ｂ 、Ｍｇ、Ｔｉ、Ｖ、Ｃｒ、Ｎｉ、Ｚｎ、
Ｇａ、Ａｓ、Ｚｒ、Ｃｅ、Ｎｄ、Ｌｉ、Ｂｅ、Ｎａ、Ｋ、Ｃａ、
Ｍｎ、Ｃｏ、Ｍｏ、Ａｇ、Ｃｄ、Ｉｎ、Ｓｎ、Ｓｂ、Ｂａ、Ｌａ、
Ｌａ、Ｐｔ、Ｈｇ、Ｐｂ、Ｂｉ、ＴｈおよびＵについて、それぞれ元素の含有量を求め、その合計量を１００％から差し引くことにより求めることができる。これらの元素の含有量は、それぞれグロー放電質量分析法により定量することができる。超高純度アルミニウム鋳塊材は、上記３７元素以外の不可避不純物を含んでいてもよい。
The purity of the ultra-high purity aluminum ingot material is expressed in mass percentage,
Fe, Si, Cu, B, Mg, Ti, V, Cr, Ni, Zn,
Ga, As, Zr, Ce, Nd, Li, Be, Na, K, Ca,
Mn, Co, Mo, Ag, Cd, In, Sn, Sb, Ba, La,
About La, Pt, Hg, Pb, Bi, Th, and U, it can obtain | require by calculating | requiring the content of an element, respectively, and subtracting the total amount from 100%. The contents of these elements can be quantified by glow discharge mass spectrometry, respectively. The ultra-high purity aluminum ingot material may contain inevitable impurities other than the 37 elements.
超高純度アルミニウム鋳塊材は、Ｓｉ、ＣｕおよびＭｇの含有量がそれぞれ１ｐｐｍ以下であることが好ましい。Ｆｅ、Ｔｉ、Ｖ、ＣｒおよびＺｒの含有量がそれぞれ０．１ｐｐｍ以下であることが好ましい。 The ultra-high purity aluminum ingot material preferably has a Si, Cu and Mg content of 1 ppm or less. The contents of Fe, Ti, V, Cr and Zr are each preferably 0.1 ppm or less.
〔熱間圧延処理〕
かかる超高純度アルミニウム鋳塊材に熱間圧延処理を施して熱間圧延材を得る。熱間圧延処理は、通常の方法、例えば加熱した鋳塊材を一対のロールの間に挟み込むことにより圧力を加えながら、これらのロール間を通過させる方法などにより施される。熱間圧延処理温度は、通常２６０℃以上６００℃以下、好ましくは３００℃以上５００℃以下である。
[Hot rolling process]
Such an ultra-high purity aluminum ingot material is subjected to a hot rolling process to obtain a hot rolled material. The hot rolling process is performed by a normal method, for example, a method of passing between these rolls while applying pressure by sandwiching a heated ingot material between a pair of rolls. The hot rolling treatment temperature is usually 260 ° C. or higher and 600 ° C. or lower, preferably 300 ° C. or higher and 500 ° C. or lower.
熱間圧延処理を施す前の超高純度アルミニウム鋳塊材の断面積(ＳH0)と、熱間圧延処理を施した後の熱間圧延材の断面積(ＳH)とから式（１）
熱間圧延加工率（％）＝［（ＳH0−ＳH）／ＳH0］×１００・・・（１）
により求められる熱間圧延加工率は、通常５０％〜９０％、好ましくは６０％〜８０％である。
熱間圧延処理は、１回で行われてもよいし、複数回に分けて繰り返し施されてもよい。
Sectional area of the ultra-high-purity aluminum ingot material before applying the hot rolling process and (S H0), the cross-sectional area of the hot rolled material was subjected to a hot rolling process (S H) Tokara formula (1)
Hot rolling ratio (%) = [(S H0 −S H ) / S H0 ] × 100 (1)
The hot rolling process rate calculated | required by (50) is 50%-90% normally, Preferably it is 60%-80%.
The hot rolling process may be performed once, or may be repeatedly performed in a plurality of times.
〔冷間圧延処理〕
熱間圧延処理により得られた熱間圧延材に、冷間圧延処理を繰り返し施す。冷間圧延処理は、通常の方法、例えば熱間圧延処理により得られた熱間圧延材を一対のロールの間に挟み込むことより圧力を加えながら、これらのロール間を通過させる方法などにより施される。
(Cold rolling process)
A cold rolling process is repeatedly performed on the hot rolled material obtained by the hot rolling process. The cold rolling treatment is performed by a normal method, for example, a method of passing between these rolls while applying pressure by sandwiching the hot rolled material obtained by the hot rolling treatment between a pair of rolls. The
冷間圧延処理における１パス加工率は３０％超４０％未満である。１パス加工率は、１回の圧延処理で圧延材に施される加工率であって、冷間圧延処理の１パス加工率は、冷間圧延処理を施す前の圧延材の断面積(Ｓ10)と、冷間圧延処理を施した後の圧延材の断面積(Ｓ1)とのから式（２）
冷間圧延加工率（％）＝［（Ｓ10−Ｓ1）／Ｓ10］×１００・・・（２）
により求められる。１パス加工率は、３０％超であり、４０％未満である。
冷間圧延処理の加工温度は６０℃以上、好ましくは６５℃以上であり、２６０℃未満、好ましくは２００℃以下である。冷間圧延処理中、大気中などへの放熱により上記加工温度を保てなくなることがあるが、このような場合には、圧延処理を一旦中断し、再度加熱してから圧延処理を再開してもよいし、外部から加熱しながら圧延処理を施してもよい。
The one-pass processing rate in the cold rolling process is more than 30% and less than 40%. The 1-pass processing rate is the processing rate applied to the rolled material in one rolling process, and the 1-pass processing rate of the cold rolling process is the cross-sectional area of the rolled material (S 10 ) and the cross-sectional area (S 1 ) of the rolled material after the cold rolling treatment, the formula (2)
Cold rolling processing rate (%) = [(S 10 −S 1 ) / S 10 ] × 100 (2)
Is required. The one pass processing rate is more than 30% and less than 40%.
The processing temperature of the cold rolling treatment is 60 ° C. or higher, preferably 65 ° C. or higher, less than 260 ° C., preferably 200 ° C. or lower. During the cold rolling process, the above processing temperature may not be maintained due to heat radiation to the atmosphere. In such a case, the rolling process is temporarily interrupted, heated again and then restarted. Alternatively, the rolling process may be performed while heating from the outside.
〔冷間圧延処理の繰り返し〕
本発明の製造方法では、上記の冷間圧延処理を繰り返し施すことにより、超高純度アルミニウム高圧延材を得る。繰り返し回数は、冷間圧延処理の１パス加工率により異なり、熱間圧延材に対する加工率が４０％超となるまで行われる。
[Repeated cold rolling process]
In the production method of the present invention, the above-described cold rolling treatment is repeated to obtain an ultra-high purity aluminum high-rolled material. The number of repetitions varies depending on the one-pass processing rate of the cold rolling process, and is performed until the processing rate for the hot-rolled material exceeds 40%.
超高純度アルミニウム高圧延材の熱間圧延材に対する加工率は、熱間圧延材の断面積(ＳH)と、得られた超高純度アルミニウム高圧延材の断面積(Ｓ)とから、式（４）
加工率（％）＝［（ＳH−Ｓ）／ＳH］×１００・・・（４）
により求められる。
The processing rate of the ultra-high purity aluminum high-rolled material to the hot-rolled material is calculated from the cross-sectional area (S H ) of the hot-rolled material and the cross-sectional area (S) of the obtained ultra-high purity aluminum high-rolled material. (4)
Processing rate (%) = [(S H −S) / S H ] × 100 (4)
Is required.
繰り返し施される冷間圧延処理の処理間隔は、３時間以内であり、好ましくは１時間以内である。処理間隔が３時間を越えると、得られる超高純度アルミニウム高圧延材は硬度が不十分なものとなり易い。 The processing interval of the cold rolling process repeatedly applied is 3 hours or less, preferably 1 hour or less. When the treatment interval exceeds 3 hours, the obtained ultra-high purity aluminum high-rolled material tends to have insufficient hardness.
〔焼鈍〕
かくして目的の超高純度アルミニウム高圧延材を得るが、得られた超高純度アルミニウム高圧延材に焼鈍処理を施してもよい。焼鈍処理は、例えば超高純度アルミニウム高圧延材を４００℃〜６００℃の温度で、１時間以上、好ましくは３時間以上、通常は２４時間以下保持することにより行われる。焼鈍処理を施すことにより、電気伝導率および熱伝導率がより高い高電気伝導・高熱伝導性超高純度アルミニウム材を得ることができる。
[Annealing]
Thus, although the intended ultra-high purity aluminum high-rolled material is obtained, the obtained ultra-high purity aluminum high-rolled material may be subjected to an annealing treatment. The annealing treatment is performed, for example, by holding the ultra-high purity aluminum high-rolled material at a temperature of 400 ° C. to 600 ° C. for 1 hour or longer, preferably 3 hours or longer, and usually 24 hours or shorter. By performing the annealing treatment, it is possible to obtain a high electrical conductivity / high thermal conductivity ultra-high purity aluminum material having a higher electrical conductivity and thermal conductivity.
〔用途〕
本発明の製造方法により得られる超高純度アルミニウム高圧延材は、例えば冷凍機、クライオポンプ、超電導マグネットなどにおいて２０Ｋ以下の極低温で使用される電気伝導体や熱伝導体などに好適に用いられる。
[Use]
The ultra-high purity aluminum high-rolled material obtained by the production method of the present invention is suitably used for electrical conductors and thermal conductors used at cryogenic temperatures of 20K or less, for example, in refrigerators, cryopumps, superconducting magnets, and the like. .
以下、実施例によって本発明の製造方法をより詳細に説明するが、本発明の製造方法は、かかる実施例によって限定されるものではない。 Hereinafter, although the manufacturing method of this invention is demonstrated in detail by an Example, the manufacturing method of this invention is not limited by this Example.
なお、各実施例において得られた高純度アルミニウム高圧延材の表面のビッカース硬度は、島津製作所社製「マイクロビッカース硬度計」を用いて荷重１００ｇの条件で測定した。 In addition, the Vickers hardness of the surface of the high-purity aluminum high-rolled material obtained in each Example was measured under the condition of a load of 100 g using a “Micro Vickers hardness meter” manufactured by Shimadzu Corporation.
実施例１
〔超高純度アルミニウム鋳塊材の鋳造〕
第１表に示す元素組成の超高純度アルミニウム〔純度９９．９９９９２％〕を黒鉛ルツボ中、真空下に７８０℃に加熱し、得られた高純度アルミニウム溶湯を鋳鉄製鋳型〔１５０℃〕に流し込んで、板状〔縦１５０ｍｍ×横２００ｍｍ×厚み２２ｍｍ〕とし、全表面を１ｍｍ深さまで研削し、縦５０ｍｍ×横５０ｍｍに切り出して厚み２０ｍｍの高純度アルミニウム鋳塊材を得た。なお、用いた高純度アルミニウム中の元素含有量は、それぞれグロー放電質量分析機〔サーモエレクトロン社製「ＶＧ９０００」〕を用いてグロー放電質量分析法により測定した。
Example 1
[Casting of ultra-high purity aluminum ingot]
Ultra high-purity aluminum (purity 99.99992%) with the elemental composition shown in Table 1 is heated to 780 ° C. in a graphite crucible under vacuum, and the resulting high-purity aluminum melt is poured into a cast iron mold [150 ° C.]. Then, it was made into a plate shape [length 150 mm × width 200 mm × thickness 22 mm], the entire surface was ground to a depth of 1 mm, and cut into length 50 mm × width 50 mm to obtain a high-purity aluminum ingot material having a thickness of 20 mm. The element content in the high-purity aluminum used was measured by glow discharge mass spectrometry using a glow discharge mass spectrometer (“VG9000” manufactured by Thermo Electron).
第 １ 表
（単位：ｐｐｍ）
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
元素 含有量 元素 含有量 元素 含有量 元素 含有量
────────────────────────────────────────
Ｓｉ ０．３７ Ｃｕ ０．１１ Ｍｇ ０．１２
────────────────────────────────────────
Ｆｅ ０．０６４ Ｔｉ ０．０３５ Ｖ ０．０３３ Ｃｒ ０．０４０
Ｚｒ ０．０２０
────────────────────────────────────────
Ｂ ０．００２ Ｎｉ ０．００３ Ｚｎ ０．００２ Ｇａ＜０．００１
Ａｓ＜０．００１ Ｃｅ＜０．００１ Ｌｉ ０．００１ Ｂｅ＜０．００１
Ｎａ＜０．００１ Ｋ ０．００８ Ｃａ ０．００９ Ｍｎ ０．００６
Ｃｏ＜０．００１ Ｍｏ ０．００３ Ａｇ＜０．００１ Ｃｄ ０．００２
Ｉｎ＜０．００１ Ｓｎ ０．００２ Ｓｂ＜０．００１ Ｂａ＜０．００１
Ｌａ＜０．００１ Ｐｔ＜０．００１ Ｈｇ ０．００２ Ｐｂ＜０．００１
Ｂｉ＜０．００１ Ｔｈ＜０．０００３ Ｕ ＜０．０００３
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
表中、Ｇａ、Ａｓ、Ｃｅ、Ｂｅ、Ｎａ、Ｃｏ、Ａｇ、Ｉｎ、Ｓｂ、Ｂａ、Ｌａ、Ｐｔ、ＰｂおよびＢｉの含有量は、それぞれ検出下限（０．００１ｐｐｍ）未満であったことを示す。ＴｈおよびＵの含有量は検出下限（０．０００３ｐｐｍ）以下であったことを示す。
Table 1
(Unit: ppm)
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
Element content Element content Element content Element content
────────────────────────────────────────
Si 0.37 Cu 0.11 Mg 0.12
────────────────────────────────────────
Fe 0.064 Ti 0.035 V 0.033 Cr 0.040
Zr 0.020
────────────────────────────────────────
B 0.002 Ni 0.003 Zn 0.002 Ga <0.001
As <0.001 Ce <0.001 Li 0.001 Be <0.001
Na <0.001 K 0.008 Ca 0.009 Mn 0.006
Co <0.001 Mo 0.003 Ag <0.001 Cd 0.002
In <0.001 Sn 0.002 Sb <0.001 Ba <0.001
La <0.001 Pt <0.001 Hg 0.002 Pb <0.001
Bi <0.001 Th <0.0003 U <0.0003
━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━━
In the table, the contents of Ga, As, Ce, Be, Na, Co, Ag, In, Sb, Ba, La, Pt, Pb, and Bi are respectively less than the lower detection limit (0.001 ppm). . It shows that the contents of Th and U were below the lower limit of detection (0.0003 ppm).
〔熱間圧延処理〕
得られた高純度アルミニウム鋳塊材に、加工温度５００℃、１パス加工率２０％の熱間圧延処理を４回繰り返し施して、熱間圧延材〔縦５２ｍｍ×横１２０ｍｍ×厚み８ｍｍ〕を得た。
[Hot rolling process]
The obtained high-purity aluminum ingot material was repeatedly subjected to hot rolling treatment at a processing temperature of 500 ° C. and a one-pass processing rate of 20% four times to obtain a hot-rolled material (length 52 mm × width 120 mm × thickness 8 mm). It was.
〔冷間圧延処理〕
得られた熱間圧延材に、室温（２５℃）雰囲気下、１２０℃〜２５０℃の温度範囲に維持しながら１パス加工率３７％の冷間圧延処理を６回施して、超高純度アルミニウム高圧延材（厚み０．５ｍｍ）を得た。冷間圧延処理の間、圧延材は、２５０℃まで加熱してから圧延処理を施し、圧延処理中に１２０℃になった時点で、直ちに圧延処理を中断し、再び２５０℃に加熱する操作を繰り返した。得られた超高純度アルミニウム高圧延材の表面のビッカース硬度を測定したところ、２５．９であった。
(Cold rolling process)
The obtained hot-rolled material was subjected to 6 cold rolling treatments with a one-pass working rate of 37% while maintaining in a temperature range of 120 ° C. to 250 ° C. in a room temperature (25 ° C.) atmosphere to obtain ultra-high purity aluminum. A highly rolled material (thickness 0.5 mm) was obtained. During the cold rolling process, the rolled material is heated to 250 ° C. and then subjected to the rolling process. When the temperature reaches 120 ° C. during the rolling process, the rolling process is immediately interrupted and the operation of heating to 250 ° C. is performed again. Repeated. It was 25.9 when the Vickers hardness of the surface of the obtained ultra-high purity aluminum high-rolled material was measured.
比較例１
冷間圧延処理の１パス加工率を６０％とし、第二冷間圧延処理の回数を３回とした以外は実施例３と同様に操作して超高純度アルミニウム高圧延材（厚み０．５ｍｍ）を得た。この超高純度アルミニウム高圧延材の表面のビッカース硬度は１７．３であった。
Comparative Example 1
The ultra-high purity aluminum high-rolled material (thickness 0.5 mm) was operated in the same manner as in Example 3 except that the one-pass processing rate of the cold rolling treatment was 60% and the number of times of the second cold rolling treatment was three. ) The Vickers hardness of the surface of this ultra-high purity aluminum high-rolled material was 17.3.
Claims (2)
得られた熱間圧延材に圧延処理を施して、該熱間圧延材に対する加工率が４０％超の超高純度アルミニウム高圧延材を製造する方法であり、
前記熱間圧延材に、
１パス加工率３０％超４０％未満で加工温度１１０℃以上２６０℃未満の冷間圧延処理
を３時間以内の処理間隔で
繰り返し施す
ことを特徴とする前記高純度アルミニウム高圧延材の製造方法。 A hot rolled material is obtained by subjecting an ultra-high purity aluminum ingot material with a purity of 99.9999% or more to a hot rolling process at a processing temperature of 260 ° C. or higher.
It is a method of subjecting the obtained hot rolled material to a rolling treatment to produce an ultra-high purity aluminum high rolled material having a processing rate of more than 40% with respect to the hot rolled material,
In the hot rolled material,
The method for producing a high-purity aluminum high-rolled material, wherein a cold rolling treatment at a machining temperature of 110 ° C. or more and less than 260 ° C. is repeatedly performed at a treatment interval of 3 hours or less at a processing rate of more than 30% and less than 40%.
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