JPS63235445A - Molybdenum wire rod and its production - Google Patents
Molybdenum wire rod and its productionInfo
- Publication number
- JPS63235445A JPS63235445A JP6920487A JP6920487A JPS63235445A JP S63235445 A JPS63235445 A JP S63235445A JP 6920487 A JP6920487 A JP 6920487A JP 6920487 A JP6920487 A JP 6920487A JP S63235445 A JPS63235445 A JP S63235445A
- Authority
- JP
- Japan
- Prior art keywords
- molybdenum
- ingot
- working
- wire rod
- processing
- 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.)
- Granted
Links
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims description 55
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- 229910052750 molybdenum Inorganic materials 0.000 claims abstract description 30
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 19
- 239000013078 crystal Substances 0.000 claims abstract description 15
- 238000005098 hot rolling Methods 0.000 claims abstract description 7
- 239000011733 molybdenum Substances 0.000 claims description 29
- FZLIPJUXYLNCLC-UHFFFAOYSA-N lanthanum atom Chemical compound [La] FZLIPJUXYLNCLC-UHFFFAOYSA-N 0.000 claims description 15
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 4
- 238000005096 rolling process Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 8
- 239000002019 doping agent Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229910052739 hydrogen Inorganic materials 0.000 description 3
- 239000001257 hydrogen Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 238000003825 pressing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 150000002751 molybdenum Chemical class 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
- Metal Rolling (AREA)
- Metal Extraction Processes (AREA)
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野］
本発明は、−膜構造材、高温炉用素材、ヒータ素材、高
温中での支持棒、ピン、ボルト等に使用されるモリブデ
ン線材とその製造方法に関する。[Detailed Description of the Invention] [Field of Industrial Application] The present invention relates to molybdenum wire rods used for membrane structural materials, materials for high temperature furnaces, heater materials, support rods in high temperatures, pins, bolts, etc. Regarding the manufacturing method.
［従来の技術］
一般に、粉末冶金法で製造されるモリブデン線及びモリ
ブデン線等を含むモリブデン線材は、純モリブデンによ
って製造され、このモリブデン線材の再結晶開始温度は
約１０００℃である。[Prior Art] Generally, molybdenum wires including molybdenum wires and molybdenum wires manufactured by powder metallurgy are manufactured from pure molybdenum, and the recrystallization start temperature of this molybdenum wire is about 1000°C.
よって、斯るモリブデンからなるモリブデン線材は、
ｔｏｏｏ℃以上の高温で使用されると、モリブデンは再
結晶粒子の成長による線部材の脆化が生じるため、高温
状態の荷重負荷に対し容易に変形してしまうという問題
があった。Therefore, the molybdenum wire made of molybdenum is
When molybdenum is used at a high temperature of 100° C. or higher, the wire member becomes brittle due to the growth of recrystallized particles, so there is a problem in that the wire member easily deforms under load at a high temperature.
そこで、高温において変形し易いという上述の欠点を補
うモリブデン材料として、従来は、アルミニウム、カリ
ウム、ケイ素等を含有したモリブデン材料が用いられて
いた。Therefore, molybdenum materials containing aluminum, potassium, silicon, etc. have been conventionally used as molybdenum materials that compensate for the above-mentioned drawback of being easily deformed at high temperatures.
［発明が解決しようとする問題点コ
しかしながら、従来のモリブデン材料は、その製造過程
において、高い加工率を必要とし、且つ。[Problems to be Solved by the Invention] However, conventional molybdenum materials require a high processing rate in the manufacturing process.
加工性が悪いために、横断面積の小さなモリブデン線材
に限られてしまうという欠点があった。Due to its poor workability, it has the disadvantage that it is limited to molybdenum wire rods with a small cross-sectional area.
そこで１本発明の目的は、上記欠点に鑑み加工性及び歩
留りに優れ、高温状態の荷重負荷に対しても、変形量の
少ない使用性の優れたモリブデン線及びモリブデン線等
のモリブデン線材を提供することである。In view of the above-mentioned drawbacks, an object of the present invention is to provide molybdenum wires and molybdenum wires that have excellent workability and yield, and are easy to use with little deformation even under high-temperature loads. That's true.
［問題点を解決するための手段］
本発明によれば、 ０．０１〜１．０重量％のランタン
又はランタン酸化物、残部がモリブデンからなり。[Means for Solving the Problems] According to the present invention, 0.01 to 1.0% by weight of lanthanum or lanthanum oxide, the balance being molybdenum.
該モリブデンの結晶粒子は実質的に繊維構造組織である
ことを特徴とする高温における変形量の少ないモリブデ
ン線材が得られる。A molybdenum wire rod with a small amount of deformation at high temperatures, which is characterized in that the molybdenum crystal particles have a substantially fibrous structure, can be obtained.
また１本発明によれば、 ０．０１〜１．０重量％のラ
ンタン又はランタン酸化物、残部がモリブデンからなる
インゴットを準備する準備工程と、該インゴットの断面
積に対して６５％以上の総加工率で加工する加工工程と
を有することを特徴とするモリブデン線材の製造方法が
得られる。According to one aspect of the present invention, there is a preparatory step of preparing an ingot consisting of 0.01 to 1.0% by weight of lanthanum or lanthanum oxide, the balance being molybdenum, and a total of 65% or more of the cross-sectional area of the ingot. There is obtained a method for manufacturing a molybdenum wire characterized by comprising a processing step of processing at a processing rate.
また、前記準備工程におけるインゴットは、当該平均粒
径が０．１〜１０ｍｍであり、前記加工工程における加
工は、熱間圧延加工、熱間転打加工、及び温間引き抜き
加工のうちから選択された少なくとも一種であることが
好ましい。Further, the ingot in the preparation step has an average grain size of 0.1 to 10 mm, and the processing in the processing step is selected from hot rolling, hot rolling, and warm drawing. It is preferable that at least one of the above be used.
すなわち１本発明によれば、モリブデン線材を製造する
場合の出発原料となるインゴットは、たとえば、 ０．
０１−１．０重量％のランタン又はランタン酸化物をド
ープしたモリブデン粉末に水素還元を施し、プレス、焼
結して形成される。このとき。That is, according to the present invention, the ingot serving as a starting material for producing a molybdenum wire rod is, for example, 0.
01-It is formed by subjecting molybdenum powder doped with 1.0% by weight of lanthanum or lanthanum oxide to hydrogen reduction, pressing, and sintering. At this time.
インゴットの結晶は、従来の２０〜５０μ腸程度の微細
な粒径を有するインゴットに比べ、ランタンのドープに
よる活性化作用により、ドープ剤を含む微小ドープ孔を
有し、且つ、結晶粒子の平均粒径が、 ０．１−１０ｍ
ｍの粗大粒となる。Compared to conventional ingots that have a fine particle size of about 20 to 50 microns, the ingot crystals have minute doping pores containing the doping agent due to the activation effect of lanthanum doping, and the average size of the crystal particles is small. Diameter is 0.1-10m
It becomes coarse grains of m.
次に、ドープ剤を含み、且つ、予め粗大化させた結晶粒
子を有する上記インゴットを、その横断面積に対して６
５％以上の加工率で熱間圧延加工。Next, the above-mentioned ingot containing a doping agent and having crystal grains coarsened in advance is
Hot rolling processing with a processing rate of 5% or more.
又は熱間転打加工、温間引き抜き加工を施して。Or by hot rolling or warm drawing.
線材の長さ方向にドープ材を配列させる。Dope material is arranged in the length direction of the wire.
これにより、第１図に示すとおり、予め粗大化した結晶
粒子は細長く成長した繊維構造組織を呈し、高温状態に
置かれた場合も等軸の微細結晶とはならない。尚、第２
図に示す通り、ランタンを含まない純モリブデンを用い
た場合のモリブデン線材では、繊維構造組織のばらつき
が見られる。As a result, as shown in FIG. 1, the crystal grains that have become coarse in advance exhibit a fibrous structure that has grown elongated, and do not become equiaxed fine crystals even when placed in a high temperature state. Furthermore, the second
As shown in the figure, when using pure molybdenum that does not contain lanthanum, molybdenum wire rods exhibit variations in fiber structure.
したがって９本発明によれば、高温状態に置かれた場合
でも、変形量の非常に少ない、高品質のモリブデン線材
が得られる。Therefore, according to the present invention, a high-quality molybdenum wire rod with very little deformation even when placed in a high temperature state can be obtained.
ここで、モリブデン線材におけるランタンの組成範囲の
限定理由について説明する。Here, the reason for limiting the composition range of lanthanum in the molybdenum wire will be explained.
ランタンをｏ、ｏｔ−ｔ、ｏ重量％添加したモリブデン
線材は、加工によって線材の長さ方向に配列したランタ
ンの粒により、粗大化したモリブデン結晶粒子は、その
線材の長さ方向に細長く成長し。Molybdenum wire rods containing o, ot-t, or o weight percent lanthanum are processed so that the lanthanum grains are arranged in the length direction of the wire, and the coarse molybdenum crystal particles grow thin and thin in the length direction of the wire. .
その直径方向には抑制される。ところが、ランタンの添
加量が、 ０．０１重量％よりも少ないと、ランタンの
ドープ剤としての効果が薄く、モリブデン結晶粒子の粒
成長の十分な抑制が困難となる。このため、高温状態に
おいてモリブデン結晶゛粒子は。It is restrained in its diametrical direction. However, when the amount of lanthanum added is less than 0.01% by weight, the effect of lanthanum as a doping agent is weak, and it becomes difficult to sufficiently suppress the grain growth of molybdenum crystal particles. Therefore, molybdenum crystal particles at high temperatures.
等軸結晶粒となり、脆化してしまう。一方、１．０重ｎ
％を越えると、多量のドープ剤の粒が生成されるため、
ｌｉ材の加工が不可能になるばかりでなく、高温状態に
おいては線材の長さ方向へのモリブデン結晶粒子の粒成
長をも抑制されてしまい。It becomes equiaxed crystal grains and becomes brittle. On the other hand, 1.0 fold n
%, a large amount of dopant particles will be produced,
Not only does it become impossible to process the Li material, but also the grain growth of molybdenum crystal grains in the length direction of the wire is suppressed at high temperatures.
却って等軸結晶粒の形成を助長してしまう結果となるか
らである。This is because, on the contrary, the formation of equiaxed crystal grains is promoted.
［実施例コ 本発明の実施例について図面を参照して説明する。[Example code] Embodiments of the present invention will be described with reference to the drawings.
まず、準備工程おいて、 ０．０１−１．０重■％のラ
ンタンをドープしたモリブデン粉末に水素還元を施し、
プレス、焼結して形成されインゴットを準備した。First, in the preparation process, molybdenum powder doped with 0.01-1.0% by weight of lanthanum is subjected to hydrogen reduction.
An ingot was prepared by pressing and sintering.
次に、加工工程において、インゴットに、その横断面積
で加工率６５％、８０％になるように圧延加工を施し、
繊維構造組織を有する棒材を形成した。Next, in the processing process, the ingot is rolled so that the processing rate is 65% and 80% in its cross-sectional area,
A rod having a fibrous structure was formed.
第３図に示すとおり、このようにして得られたモリブデ
ン線材から、 ３ ｔ Ｘ１０Ｘ１２０ ａｍの試片
を作成し、これら試片上に約１．０ｋｇの荷重を載せて
。As shown in FIG. 3, specimens of 3 t x 10 x 120 am were prepared from the molybdenum wire obtained in this manner, and a load of approximately 1.0 kg was placed on these specimens.
水素雰囲気中の電気炉内で、 １７００℃、 １０時間
加熱する変形試験をおこなった。A deformation test was conducted in an electric furnace in a hydrogen atmosphere at 1700°C for 10 hours.
その結果を表１に掲げる。尚、比較例として。The results are listed in Table 1. As a comparative example.
純モリブデンからなるインゴットを用いて製造されたモ
リブデン線材の変形試験結果（ａ、ｂ）を表の下段に示
す。The results of deformation tests (a, b) of molybdenum wire manufactured using ingots made of pure molybdenum are shown in the lower part of the table.
その結果１表１に示されるとおり、ランタンを０．０１
−１．０％含有させた本発明に係わるモリブデン棒材（
１〜６）は、変形量が極めて少ないことが認められる。As shown in Table 1, the results showed that 0.01
- Molybdenum rod according to the present invention containing 1.0% (
1 to 6), it is recognized that the amount of deformation is extremely small.
次に、室温での脆化を調べる為１本発明に係る０、５％
ランタン含含有モリブデン色、比較例として純モリブデ
ンからなる試片（！０φＸ９０ｍｍ）とを、１８００℃
ＸＩＯ時間加熱後、万能試験機を使用し、試験スピード
１ ｓ＋ａｌ／ｍｌｎ＋ スパン５０ｍ１ｍで三点曲
げ試験を行った。Next, in order to examine embrittlement at room temperature, 0.5% according to the present invention
Molybdenum color containing lanthanum, and a sample made of pure molybdenum (!0φX90mm) as a comparative example, was heated at 1800℃.
After heating for XIO hours, a three-point bending test was conducted using a universal testing machine at a test speed of 1 s+al/mln+ and a span of 50 ml/m.
その結果、第４図に示すとおり１本発明に係るモリブデ
ン棒材では、９０°曲げにも十分耐え得ることが認めら
れた。一方、比較例の純モリブデンより作成された試片
は１曲げ角Ｏ＠で簡単に破壊した。As a result, as shown in FIG. 4, it was found that the molybdenum bar according to the present invention could sufficiently withstand bending at 90°. On the other hand, a specimen made of pure molybdenum as a comparative example was easily broken at a bending angle of 1°.
［発明の効果コ
以上の説明のとおり９本発明によれば、 ０．０１〜１
．０重量％のランタンのドープにより予め粗大化させた
結晶粒子を有するインゴットを、その断面積に対して６
５％以上の加工率で加工を施して、ドープ剤をモリブデ
ン線材の長さ方向に配列させることにより、実際の使用
中の高温杖態において。[Effects of the Invention] As explained above, 9 According to the present invention, 0.01 to 1
．． An ingot having crystal grains coarsened in advance by doping with 0% by weight of lanthanum is
By processing at a processing rate of 5% or more and arranging the dopant in the length direction of the molybdenum wire, it can be used in the form of a high-temperature rod during actual use.
線材の直径方向への粒成長が抑制され、その長さ方向に
細長く粒成長した繊維構造組織を有するモリブデン線材
が得られるから、加工性及び歩留りに優れ、高温状態の
荷重負荷に対しても、変形量の少ない使用性の優れたモ
リブデン線材とその製造方法を提供することができる。Grain growth in the diameter direction of the wire is suppressed, and a molybdenum wire with a fibrous structure with elongated grain growth in the length direction is obtained, so it has excellent workability and yield, and can withstand loads under high temperature conditions. It is possible to provide a molybdenum wire rod with a small amount of deformation and excellent usability, and a method for manufacturing the same.
【図面の簡単な説明】
第１図は本発明の実施例に係る圧延加工率９８．７％の
モリブデン線材の繊維構造Ｍ織を示す断面図（×５０倍
）、第２図は従来のランタンを含まない純モリブデンを
用いた圧延加工率９８．７％のモリブデン棒材の構造組
織を示す断面図（×５０倍）、第３図は変形試験の略図
、第４図は三点曲げ試験の結果を示す断面図である。
１・・・試片、２・・・荷１゜
Ｕ）
〜
Ｕ）
×
第３図
第４図
手続：？′Ｆｔ１正書（自発）
昭和６３年６月１８日
許庁長官 吉田文毅殿
６事件の表示
昭和６２年特許願第６９２０４号
２、発明の名称
モリブデン線材とその製造方法
３、補正をする者[Brief Description of the Drawings] Figure 1 is a cross-sectional view (x50x) showing a fiber structure M weave of a molybdenum wire rod with a rolling reduction rate of 98.7% according to an embodiment of the present invention, and Figure 2 is a cross-sectional view of a conventional lantern. A cross-sectional view (x50x) showing the structural structure of a molybdenum bar with a rolling reduction rate of 98.7% using pure molybdenum containing no FIG. 3 is a cross-sectional view showing the results. 1...Special piece, 2...Load 1゜U) ~ U) × Figure 3 Figure 4 Procedure:? 'Ft1 official manuscript (spontaneous) June 18, 1988 Commissioner of the License Agency Bunki Yoshida Indication of the 6 case 1988 Patent Application No. 69204 2 Title of the invention Molybdenum wire rod and its manufacturing method 3 Person making the amendment
Claims (1)
化物、残部がモリブデンからなり、該モリブデンの結晶
粒子は実質的に繊維構造組織であることを特徴とする高
温における変形量の少ないモリブデン線材。 ２）０、０１〜１．０重量％のランタン又はランタン酸
化物、残部がモリブデンからなるインゴットを準備する
準備工程と、該インゴットの断面積に対して６５％以上
の総加工率で加工する加工工程とを有することを特徴と
するモリブデン線材の製造方法。 ３）特許請求の範囲第２項記載のモリブデン線材の製造
方法において、前記準備工程におけるインゴットは、当
該平均粒径が０．１〜１０ｍｍであることを特徴とする
モリブデン線材の製造方法。 ４）特許請求の範囲第２項又は第３項記載のモリブデン
線材の製造方法において、前記加工工程における加工は
、熱間圧延加工、熱間転打加工、及び温間引き抜き加工
のうちから選択された少なくとも一種であることを特徴
とするモリブデン線材の製造方法。[Scope of Claims] 1) A high-temperature device comprising 0.01 to 1.0% by weight of lanthanum or lanthanum oxide, the remainder being molybdenum, and the crystal particles of the molybdenum having a substantially fibrous structure. A molybdenum wire rod with a small amount of deformation. 2) Preparation step of preparing an ingot consisting of 0.01 to 1.0% by weight of lanthanum or lanthanum oxide, the balance being molybdenum, and processing at a total processing rate of 65% or more with respect to the cross-sectional area of the ingot. A method for producing a molybdenum wire, comprising the steps of: 3) The method for producing a molybdenum wire according to claim 2, wherein the ingot in the preparation step has an average particle size of 0.1 to 10 mm. 4) In the method for manufacturing a molybdenum wire rod according to claim 2 or 3, the processing in the processing step is selected from hot rolling processing, hot rolling processing, and warm drawing processing. 1. A method for producing a molybdenum wire, characterized in that at least one type of molybdenum wire is used.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6920487A JPS63235445A (en) | 1987-03-25 | 1987-03-25 | Molybdenum wire rod and its production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6920487A JPS63235445A (en) | 1987-03-25 | 1987-03-25 | Molybdenum wire rod and its production |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63235445A true JPS63235445A (en) | 1988-09-30 |
| JPH0320456B2 JPH0320456B2 (en) | 1991-03-19 |
Family
ID=13395961
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6920487A Granted JPS63235445A (en) | 1987-03-25 | 1987-03-25 | Molybdenum wire rod and its production |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63235445A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110605398A (en) * | 2019-10-11 | 2019-12-24 | 北京北钨科技有限公司 | Preparation method of lanthanum-micro-doped high-temperature molybdenum wire |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59177345A (en) * | 1983-03-29 | 1984-10-08 | Toshiba Corp | Molybdenum for structural material |
-
1987
- 1987-03-25 JP JP6920487A patent/JPS63235445A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59177345A (en) * | 1983-03-29 | 1984-10-08 | Toshiba Corp | Molybdenum for structural material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110605398A (en) * | 2019-10-11 | 2019-12-24 | 北京北钨科技有限公司 | Preparation method of lanthanum-micro-doped high-temperature molybdenum wire |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0320456B2 (en) | 1991-03-19 |
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