JPS59177345A - Molybdenum for structural material - Google Patents
Molybdenum for structural materialInfo
- Publication number
- JPS59177345A JPS59177345A JP5145483A JP5145483A JPS59177345A JP S59177345 A JPS59177345 A JP S59177345A JP 5145483 A JP5145483 A JP 5145483A JP 5145483 A JP5145483 A JP 5145483A JP S59177345 A JPS59177345 A JP S59177345A
- Authority
- JP
- Japan
- Prior art keywords
- molybdenum
- particle size
- grain size
- la2o3
- structural material
- 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
Abstract
Description
【発明の詳細な説明】
〔発明の技術分野」
本発明は、Ｌａ２０．粒子がＭｏ中に均一に分散された
措造材料用のモリブデンに関する。DETAILED DESCRIPTION OF THE INVENTION [Technical Field of the Invention] The present invention relates to La20. The present invention relates to molybdenum for use in construction materials in which particles are uniformly dispersed in Mo.
Ｌａ、Ｏ，，全含有せるＭｏ材は、主に電子管の陰極材
として、コイル状（スパイラル状）の′Ｉａまたは板を
丸めた円筒とし、て供される。A Mo material containing all of La, O, etc. is mainly used as a cathode material for an electron tube in the form of a coiled (spiral) Ia or a cylinder formed by rolling a plate.
ところで、Ｍｏ中のしａ２０ｓ ｉ！酸化トリウム入り
タングステン（ＴｈＯ□−Ｗ）中のＴｈｅ２と同様にＭ
Ｏと固溶したシ化合物を形底することなく、Ｍｏ中にＬ
ａ２０゜の粒子として分散されている。By the way, Mochu's a20s i! Similar to The2 in tungsten containing thorium oxide (ThO□-W), M
L in Mo without forming a solid solution of silica compound with O.
It is dispersed as particles of a20°.
このため、このようなモリブデン材料の諸物件は、Ｌａ
２Ｏ５粒子の含有量のみならず、その分散状態の影響を
大きく受ける。For this reason, such properties of molybdenum materials are
It is greatly influenced not only by the content of 2O5 particles but also by their dispersion state.
例えば、Ｍｏ中のＬａ、０３が凝集している等、Ｌａ２
Ｏ３粒子の分散状態が悪い場合にはコイル状あるいは円
筒状に賦形する等の二次加工を施す、際に、しばしば断
線したシ、亀裂を生じるという問題が生じた。For example, La203 in Mo is aggregated, etc.
If the O3 particles are poorly dispersed, there is a problem that wire breaks and cracks often occur during secondary processing such as shaping into a coil or cylinder.
また、上記の如（Ｍｏ中のＬａ２Ｏ３の分散状態が悪い
と、電子管の陰極材として用いた場合には良好な電子放
出特性が得られにくく、しかも短寿命となるという種々
の問題があった。Further, as mentioned above, if the dispersion state of La2O3 in Mo is poor, it is difficult to obtain good electron emission characteristics when used as a cathode material for an electron tube, and there are various problems such as short life.
しかしながら、従来、モリブデン材料に添加すべきＬ
ａ２０ｓの適切な分散状態が知られていなかつ／こため
、上記加工性、電子放射特性などの諸問題を解決するこ
とができなかった。However, conventionally, L to be added to molybdenum materials
Since the appropriate dispersion state of a20s is not known and/or therefore, various problems such as processability and electron emission characteristics cannot be solved.
本発明の目的に１、上記問題点を解消し、構造材として
用いた場合には容易に二次加工ができ、しかもＴＩＣ子
管０陰極相として用いた場合には長寿命となるＬａ、０
３を１〜５ ｉｆ（量多含有するＭｏ材を提供すること
にある。The purpose of the present invention is to solve the above-mentioned problems, and when used as a structural material, it can be easily subjected to secondary processing, and when used as a TIC subtube 0 cathode phase, it has a long life.
The object of the present invention is to provide a Mo material containing a large amount of 3 if 1 to 5 if.
本発明者らは上記目的を達成すべく、鋭意研死を重ねた
結果、Ｌａ２０．を１〜５．＠量チ含有するＭ。The inventors of the present invention have worked diligently to achieve the above object, and as a result, La20. 1 to 5. @M containing quantity.
材において、Ｍｏ中にＬａ２０，１粒子を均一かつ做細
に分散せしめると、その二次加工性、電子放出特性等の
緒特性が改善されることを見出し、本発明を完成した。The present invention was completed based on the discovery that when La20,1 particles are uniformly and finely dispersed in Mo, the secondary processability, electron emission properties, and other properties of the material are improved.
木兄ψ」の構造材用モリブデンは、モリブデン（Ｍｏ）
中にｉ 〜５４ｆｉ Ｑ ％の酸化ランタン（Ｌａ２Ｏ
３）が均一に分散されており、該分散された酸化ランタ
ン（Ｌａ２Ｏ５）の個々の平均粒径が３ｔ１ｍ以下であ
って、かつ、最大粒径が７μｍ以下であることを本発明
において、Ｌａ２Ｏ５は電子放出能を与え、かつ、高温
強度を高める成分である。The molybdenum used in the structural material of ``KIEN ψ'' is molybdenum (Mo).
i~54fiQ% of lanthanum oxide (La2O
In the present invention, La2O5 is homogeneously dispersed, and the individual average particle size of the dispersed lanthanum oxide (La2O5) is 3t1m or less, and the maximum particle size is 7μm or less. It is a component that provides electron-emitting ability and increases high-temperature strength.
Ｌａ２０．の含有量は１〜５重量％とする。Ｌａ２Ｏ３
の含有量が１−未満の場合はＬａ２ｏ３の添加効果が得
られにくく、純Ｍｏに近い特性を示し、５％を超えた場
合は、５％以下の添加効果と、さほど大きな変化が認め
られず、しかも、二次加工性が悪くなる等の問題点を生
じる。La20. The content is 1 to 5% by weight. La2O3
If the content is less than 1-, it is difficult to obtain the effect of adding La2o3, and it exhibits properties close to pure Mo, and if it exceeds 5%, the effect of adding La2o3 is less than 5%, and no significant change is observed. Moreover, problems such as poor secondary workability occur.
Ｌ ａ２０３の粒子径は平均粒径て３μＩｎ以下であり
、かつ、最大粒径で７μｍ以下でなりればならない。The particle size of La203 must be an average particle size of 3 μIn or less and a maximum particle size of 7 μm or less.
平均粒径が３μｒｎｆ超えるか、または、最大粒径が７
μｍｆ：超えると、線または板を二次加工する際に断線
したり、亀裂が入る等、著しるしく加工性が低下するば
かりでなく、ｉｔ子管の陰極材料として用いた場合、長
時間安定な電子放出特性を得ることが困難となる。The average particle size exceeds 3 μrnf or the maximum particle size is 7
μmf: If it exceeds, not only will the wire or plate be broken or cracked during secondary processing, resulting in a marked decrease in workability, but it will also be stable for a long time when used as a cathode material for an IT tube. It becomes difficult to obtain suitable electron emission characteristics.
更に、線あるいは板材の二次加工性は、Ｌａ２Ｏ３の含
有量、分散形態の他に、モリブデン（ＭＯ）と酸化ラン
タン（Ｌａ２Ｏ５）からなる焼結体からの加工率（１ｒ
１Ｐｉ、断面積の変化￥′、）に形管されろ。Furthermore, the secondary workability of a wire or plate material is determined by the processing rate (1 r
1Pi, change in cross-sectional area \',).
木兄Ｑｌの構造利用モリブデンｋｔ、好ましくは１、チ
２（１結体からの加工率６０係以上で加工でれたもので
ある。Ｍｏの様に、もともとＣｕ 、 Ａ７−ｊと比較
して脆い金属に１：、焼結によって生じる方向性のない
結晶組織を、力ｎ工することによって、その加工方向に
配向した結晶組織を形成させることができる。Structural utilization of Molybdenum KT, preferably 1, 2 (processed from 1 solid at a processing rate of 60 or more. Like Mo, originally Cu, compared to A7-j) By subjecting a brittle metal to a non-directional crystal structure produced by sintering, it is possible to form a crystal structure oriented in the working direction.
このような集合組ｏｆ：形成させることによって溝端材
用モリブデンの柔軟性が向上する。Ｌａ２Ｏ３１〜５Ｍ
量チ含有せるＮｏ材において、発明者の実験結果によれ
は、焼結体からの加工率は、太きくなる程二次加工性が
容易となるが、６０チ以上の加工率を有する線、あるい
は仮相であれば、笑用上問題ない８
し発明の実施例」
以下本発明のＬａ２０３１〜５蕉針係含イｊせるＩＶＩ
。By forming such a set of sets, the flexibility of the molybdenum for the groove end material is improved. La2O31~5M
According to the inventor's experimental results, in No material containing a quantity of 60 mm, the machining rate from the sintered body becomes easier as the thickness increases, but the line with a machining rate of 60 mm or more, Or, if it is a temporary form, there is no practical problem.
.
イ１の特徴を説、明する。Explain and explain the characteristics of A1.
粉末冶金法によってＬａ２Ｏ５含有預を０．５ 、１．
０ 。By powder metallurgy method, the La2O5 content is 0.5, 1.
0.
２．０ 、４．０ 、６．０７ＥＴ、ｆ、Ｊ％、さらに
： Ｌａ２９３粒径に差が出る様、添加慧、混合方法を
変え、機械プレスによｌ） １．５ ｔｏｎ／ｙ＋Ｊの
圧力で圧粉体を作り、この圧粉体を１８５０℃で８時間
水素雰囲気中で焼結した。この時得られた焼結体は、比
重が約９．５０、断面が１２Ｘ１２鰭、長さ６５０飼の
形状であった。この焼結体を温度を加えなから転打加工
、引抜き加工を施し、０．６０ ｔｔｒｍφの線を得た
。Ｍｏ線中のＬ８２０３粒子径の確認は、ｍ’を熱硬化
性樹脂の中に埋込み、通常の研磨法にょシ鏡面仕上後、
特殊な電解研磨法によｔ） Ｍｏ材のみを研磨しｓ Ｌ
ｌ、０ｓ１ｒ。2.0, 4.0, 6.07ET, f, J%, and further: In order to make a difference in La293 particle size, the addition temperature and mixing method were changed, and a pressure of 1.5 ton/y + J was applied using a mechanical press. A green compact was produced, and this green compact was sintered at 1850° C. for 8 hours in a hydrogen atmosphere. The sintered body obtained at this time had a specific gravity of about 9.50, a cross section of 12×12 fins, and a length of 650 fins. This sintered body was subjected to rolling processing and drawing processing without applying any temperature to obtain a wire having a diameter of 0.60 ttrmφ. To confirm the particle size of L8203 in the Mo wire, m' was embedded in a thermosetting resin, and after mirror finishing using the usual polishing method,
Only the Mo material is polished using a special electrolytic polishing method.
l, 0s1r.
研磨面に浮き上がらせる様に残留させた後、走査型電子
顕微鏡によシ観察した。After leaving it to float on the polished surface, it was observed using a scanning electron microscope.
線径０．６０ ｍｈφにおけるＭｏ中のＬ ａ（０３含
有量及び＋ Ｌａ、０．の最大粒子径と線の柔軟性、二
次再結晶温度との関連を第１表に示した。Table 1 shows the relationship between the maximum particle diameter of La (03 content and + La, 0.) in Mo with a wire diameter of 0.60 mhφ, wire flexibility, and secondary recrystallization temperature.
これから明らかな如く、Ｌａ２０．、の含有量は１．０
〜５重量％が最も良く、本発明者らの実験結果によれば
２〜３重量％が最も適正な量である。又、Ｌａ、Ｏ，、
の粒子径は小さい方が良く、８μｍを超えると二次加工
性は急激に低下する。As is clear from this, La20. , the content of is 1.0
~5% by weight is the best amount, and according to the experimental results of the present inventors, the most appropriate amount is 2 to 3% by weight. Also, La, O,...
The smaller the particle size, the better; if it exceeds 8 μm, the secondary processability will drop sharply.
また、上記圧粉体を２ ｔｏｎ％−の静水圧でプレスし
、圧粉体を成形し、水素雰囲気中にて１８５０℃×８時
間焼結して得られた比重９．４５、直径６０晒φ、長さ
４００閣の形状の焼結体を・・ンマー加工、ロール加工
し厚さ帆２−の板を得た。この時、中間で、水素雰囲気
中にて二次再結晶温度以上で熱処理した。熱処理する板
材の寸法は、弾厚帆２間に加工する迄の加工率が４０％
、６０％、８０チとした。この時の板材の柔軟性につい
て調査した結果を第２表に示す。In addition, the above green compact was pressed with a hydrostatic pressure of 2 ton% to form a green compact, and the green compact was sintered in a hydrogen atmosphere at 1850°C for 8 hours, with a specific gravity of 9.45 and a diameter of 60. A sintered body in the shape of φ and 400 mm in length was processed and rolled to obtain a plate with a thickness of 2 mm. At this time, in the middle, heat treatment was performed in a hydrogen atmosphere at a temperature equal to or higher than the secondary recrystallization temperature. The dimensions of the plate material to be heat treated are such that the processing rate is 40% before processing between the two bullet sails.
, 60%, and 80chi. Table 2 shows the results of an investigation regarding the flexibility of the plate material at this time.
この結果から明らかな如く６０チ以上加工を施工された
板材の柔軟性が艮いことがわかる加工率による柔軟性効
果（徒、線の場合もまったく同様である。As is clear from these results, it is clear that the flexibility of the plate material processed with 60 or more wires is remarkable.
次に電力管（細径０．２ｎ＋ｍφ）を用いＭＯ中のＬａ
２Ｏ３含有量と、１に子放出特性との関連性を第３表に
示す。第３岩によると、Ｌ ａ２０３の含有量は１．０
重量チ以上必要であり、６．０重量％を超えても電子放
出特性は良くならず、むしろ２１Ｆ量係の弱性に比較し
て若干、低下傾向がある。Next, use a power tube (small diameter 0.2n+mφ) to
Table 3 shows the relationship between the 2O3 content and the particle release characteristics. According to the third rock, the content of La203 is 1.0
It is necessary to use more than 6.0% by weight, and even if it exceeds 6.0% by weight, the electron emission characteristics do not improve, but rather tend to deteriorate slightly compared to the weakness of the 21F content.
第 ３ 表
し本発明の効果〕
Ｊ２ノ上の嘘、明から明らかな様に本発明の構造材用モ
リブデンは、
■その二次加工性が良好であること、■二次再結晶温度
が高く、従って高温強度が高いこと、■電子放出特性が
安定で、かつ、優れること等の効果を奏し、その工業的
価値は極めて大でろふ。3. Effects of the present invention] J2 As is clear from the above, the molybdenum for structural materials of the present invention has the following properties: ■ its secondary processability is good; ■ its secondary recrystallization temperature is high; Therefore, it has effects such as high high-temperature strength and stable and excellent electron emission properties, and its industrial value is extremely large.
Claims (1)
ンメン（Ｌａ２ｏ、 ）が均一に分散されておシ、該分
散された酸化ランタン（Ｌａ、０． ）の個々の平均粒
径が３μｍ以下であって、かつ、最大粒径が７μｍ以下
であること￥％徴とする構造利用モリブデン。 ２ モリブデン（Ｍｏ）粉末と酸化ランタン（Ｌａ２０
ｇ）とからなる焼結体に加工率６０チ以上の加工を施し
て成る特許請求の範囲第１項記載の構造利用モリブデン
。[Claims] 1 Molybdenum (84o) has 1 to 5 heavy weight oxides (La2o, ) uniformly dispersed therein, and each of the dispersed lanthanum oxides (La, 0. Structural molybdenum with an average particle size of 3 μm or less and a maximum particle size of 7 μm or less. 2 Molybdenum (Mo) powder and lanthanum oxide (La20
The structurally utilized molybdenum according to claim 1, which is obtained by processing a sintered body comprising g) at a processing rate of 60 inches or more.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5145483A JPS59177345A (en) | 1983-03-29 | 1983-03-29 | Molybdenum for structural material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5145483A JPS59177345A (en) | 1983-03-29 | 1983-03-29 | Molybdenum for structural material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS59177345A true JPS59177345A (en) | 1984-10-08 |
| JPS6237707B2 JPS6237707B2 (en) | 1987-08-13 |
Family
ID=12887375
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5145483A Granted JPS59177345A (en) | 1983-03-29 | 1983-03-29 | Molybdenum for structural material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59177345A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63157832A (en) * | 1986-12-19 | 1988-06-30 | Tokyo Tungsten Co Ltd | Molybdenum plate and its production |
| JPS63192850A (en) * | 1987-02-05 | 1988-08-10 | Tokyo Tungsten Co Ltd | Molybdenum plate and its production |
| JPS63235445A (en) * | 1987-03-25 | 1988-09-30 | Tokyo Tungsten Co Ltd | Molybdenum wire rod and its production |
| JPS63238237A (en) * | 1987-03-25 | 1988-10-04 | Tokyo Tungsten Co Ltd | Molybdenum wire rod and its production |
| JPH01502680A (en) * | 1987-01-28 | 1989-09-14 | メタルウエルク、プランゼー、ゲゼルシヤフト、ミツト、ベシユレンクテル、ハフツング | Creep-resistant alloy made of high-melting point metal and its manufacturing method |
| US5134039A (en) * | 1988-04-11 | 1992-07-28 | Leach & Garner Company | Metal articles having a plurality of ultrafine particles dispersed therein |
| CN111187958A (en) * | 2020-02-19 | 2020-05-22 | 西安交通大学 | Mo powder/MoO2Method for preparing nano lanthanum-molybdenum oxide alloy by doping with lanthanum molybdate amine powder |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0518650Y2 (en) * | 1987-09-22 | 1993-05-18 |
-
1983
- 1983-03-29 JP JP5145483A patent/JPS59177345A/en active Granted
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63157832A (en) * | 1986-12-19 | 1988-06-30 | Tokyo Tungsten Co Ltd | Molybdenum plate and its production |
| JPH0549736B2 (en) * | 1986-12-19 | 1993-07-27 | Tokyo Tungsten Kk | |
| JPH01502680A (en) * | 1987-01-28 | 1989-09-14 | メタルウエルク、プランゼー、ゲゼルシヤフト、ミツト、ベシユレンクテル、ハフツング | Creep-resistant alloy made of high-melting point metal and its manufacturing method |
| JPS63192850A (en) * | 1987-02-05 | 1988-08-10 | Tokyo Tungsten Co Ltd | Molybdenum plate and its production |
| JPH0238659B2 (en) * | 1987-02-05 | 1990-08-31 | Tokyo Tungsten Kk | |
| JPS63235445A (en) * | 1987-03-25 | 1988-09-30 | Tokyo Tungsten Co Ltd | Molybdenum wire rod and its production |
| JPS63238237A (en) * | 1987-03-25 | 1988-10-04 | Tokyo Tungsten Co Ltd | Molybdenum wire rod and its production |
| JPH0320456B2 (en) * | 1987-03-25 | 1991-03-19 | Tokyo Tungsten Kk | |
| JPH0322460B2 (en) * | 1987-03-25 | 1991-03-26 | Tokyo Tungsten Kk | |
| US5134039A (en) * | 1988-04-11 | 1992-07-28 | Leach & Garner Company | Metal articles having a plurality of ultrafine particles dispersed therein |
| CN111187958A (en) * | 2020-02-19 | 2020-05-22 | 西安交通大学 | Mo powder/MoO2Method for preparing nano lanthanum-molybdenum oxide alloy by doping with lanthanum molybdate amine powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS6237707B2 (en) | 1987-08-13 |
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