JPS63166952A - Manufacture of molybdenum material - Google Patents
Manufacture of molybdenum materialInfo
- Publication number
- JPS63166952A JPS63166952A JP31132286A JP31132286A JPS63166952A JP S63166952 A JPS63166952 A JP S63166952A JP 31132286 A JP31132286 A JP 31132286A JP 31132286 A JP31132286 A JP 31132286A JP S63166952 A JPS63166952 A JP S63166952A
- Authority
- JP
- Japan
- Prior art keywords
- temperature
- heat treatment
- bar
- wire
- swaging
- 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
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 title claims description 19
- 229910052750 molybdenum Inorganic materials 0.000 title claims description 7
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 title claims description 5
- 239000011733 molybdenum Substances 0.000 title claims description 5
- 238000010438 heat treatment Methods 0.000 claims abstract description 27
- 238000001953 recrystallisation Methods 0.000 claims abstract description 13
- 238000005491 wire drawing Methods 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 5
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 5
- 239000002019 doping agent Substances 0.000 claims abstract 2
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000005096 rolling process Methods 0.000 claims 1
- 239000007787 solid Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000000843 powder Substances 0.000 abstract description 4
- 239000006104 solid solution Substances 0.000 abstract description 4
- 229910052804 chromium Inorganic materials 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 229910052736 halogen Inorganic materials 0.000 description 12
- 150000002367 halogens Chemical class 0.000 description 12
- 238000012360 testing method Methods 0.000 description 12
- 238000012545 processing Methods 0.000 description 11
- 239000013078 crystal Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 230000007423 decrease Effects 0.000 description 5
- 239000011888 foil Substances 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007665 sagging Methods 0.000 description 3
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000002159 abnormal effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000012733 comparative method Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000002207 thermal evaporation Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Landscapes
- Powder Metallurgy (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
この発明は高温強度にすぐれ、且つ高温炭熱処理後常温
における耐脆性にもすぐれたＭｏ材の製造方法に関する
。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a method for producing a Mo material that has excellent high-temperature strength and excellent brittle resistance at room temperature after high-temperature coal heat treatment.
炉用ヒータや蒸着用ボートなどの高温下で使用されてい
るモリブデン材枠（以下Ｍｏ材と言う）としてはＱｌ、
Ｓｉ、ＫをドープしたＭｏ材があり、常温における高伸
性のＭｏ材にはＰｅ、 Ｎｉ、 Ｇｏ、 Ｃｒなどを固
溶させたものがある。Molybdenum material frames (hereinafter referred to as Mo materials) used under high temperature conditions such as furnace heaters and vapor deposition boats include Ql,
There are Mo materials doped with Si and K, and Mo materials with high elongation at room temperature include those in which Pe, Ni, Go, Cr, etc. are dissolved in solid solution.
これらのＭｏ材は従来、マンドレル、アンカー、サポー
ト、Ｍｏ箔材などに使用されている。そしてこれらの使
用態様は比較的低い温度、例えば再結晶温度以下であっ
た。このＭｏ材が、ＪＩＳ Ｈ４タイプの自動車用のハ
ロゲンランプに使われるＭｏサポートとして使用される
例を第１図により説明する。These Mo materials have conventionally been used for mandrels, anchors, supports, Mo foil materials, etc. And these usage modes were at relatively low temperatures, for example, below the recrystallization temperature. An example in which this Mo material is used as a Mo support for a JIS H4 type automobile halogen lamp will be explained with reference to FIG.
ランプ中にＡｒガスとＢｒｚ又はＣ）１．Ｂｒガスにご
く少量のＨ２ガスを封入する。図において１は石英又は
硬質ガラスランプである。２．４はＷフィラメント、５
はＭｏサポート上に６のＭｏスリーブが溶接され、Ｍｏ
スリーブを通してＷフィラメントの各々の足がかしめ止
められている。また、３はＭＯミラーでその一端にＭｏ
スリーブが溶接され、１のフィラメントの片側の足がか
しめ止められている。また、５のＭｏサポートは、８の
Ｍｏ箔を介して外側のＭｏサポート７に連結している。Ar gas and Brz or C)1. A very small amount of H2 gas is enclosed in Br gas. In the figure, 1 is a quartz or hard glass lamp. 2.4 is W filament, 5
6 Mo sleeves are welded onto the Mo support, and the Mo
Each leg of the W filament is crimped through the sleeve. In addition, 3 is an MO mirror with Mo
The sleeve is welded and one leg of filament 1 is caulked. Moreover, the Mo support 5 is connected to the outer Mo support 7 via the Mo foil 8.
一方、７のＭｏサポートはＦｅ−Ｎｉリード線に溶接さ
れ連結している。On the other hand, the Mo support No. 7 is welded and connected to the Fe-Ni lead wire.
第１図のハロゲン電球において、Ｗフィラメントは凡そ
２８００℃以上の高温度で点灯されているが、封入ガス
中のＢｒｚによりＷ ＋ Ｂｒｚ ４ＷＢｒ２の如きＷ
の再生ハロゲンサイクルによりタングステンが蒸発して
もＢｒｚガスによりＷＢｒｚが形成され、それがハロゲ
ンサイクルにより再び分解してＷフィラメント上にＷが
析出する。このことによりＷフィラメントの劣化は著し
く抑制されるという原理であるが、実際はＷとＢｒｚの
反応は可逆反応であるのでＷがある一定量蒸発すると球
内のＷＢｒｇとの間に平衡関係が生まれＷフィラメント
の蒸発を抑制する。このメカニズムによって高効率、高
寿命のハロゲンランプが得られる。In the halogen light bulb shown in Figure 1, the W filament is lit at a high temperature of approximately 2800°C or higher, but due to Brz in the filled gas, W such as W + Brz 4WBr2
Even if tungsten evaporates during the regenerating halogen cycle, WBrz is formed by the Brz gas, which is decomposed again during the halogen cycle, and W is deposited on the W filament. The principle is that the deterioration of the W filament is significantly suppressed by this, but in reality, the reaction between W and Brz is a reversible reaction, so when a certain amount of W evaporates, an equilibrium relationship is created between WBrg in the sphere and WBrz. Suppress filament evaporation. This mechanism provides a halogen lamp with high efficiency and long life.
既述の如く、Ｗフィラメントの蒸発の抑制はＷの再生ハ
ロゲンサイクルによるが、その反応を円滑にするために
フィラメント近傍の外壁温度は凡そ７００℃程度の温度
に保持されていなければならないが、激しく蒸発して球
の黒化現象を併発して効率は低下して短寿命となる。As mentioned above, the suppression of evaporation of the W filament is due to the W regeneration halogen cycle, but in order to make the reaction smooth, the temperature of the outer wall near the filament must be maintained at approximately 700°C, but the Evaporation causes the bulb to darken, reducing efficiency and shortening its lifespan.
外壁の温度が異常となる原因はタングステン線とモリブ
デンサポートの耐垂下性に起因する。タングステン線に
関する耐垂下性はハロゲンランプ用として改良が加えら
れているが、Ｍｏサポートについてはこれまで余り問題
にされてなかったが最近は、Ｍｏサポートの耐垂下性（
耐変形性ともいう）がＷと同様に重要であることが判っ
た。“本発明は既述、１項において得られた材料を更に
粗大結晶化開始温度の１００℃以上において、ハロゲン
ランプ用に組立てる前に加熱処理することによって”、
使用中に繊維構造より粗大結晶化する過程において生ず
る変形をあらかじめ除去することによってＭｏサポート
の変形を防止して、Ｗの再生ハロゲンサイクルを正常化
する。The reason why the temperature of the outer wall becomes abnormal is due to the sagging resistance of the tungsten wire and molybdenum support. The sagging resistance of tungsten wire has been improved for use in halogen lamps, but Mo supports have not been much of an issue until now, but recently the sagging resistance of Mo supports (
It was found that deformation resistance (also called deformation resistance) is as important as W. “The present invention is achieved by further heat-treating the material obtained in Section 1 above at 100°C or higher, the temperature at which coarse crystallization begins, before assembling it into a halogen lamp.”
By removing in advance the deformation that occurs during the process of coarse crystallization from the fiber structure during use, deformation of the Mo support is prevented and the regeneration halogen cycle of W is normalized.
また、第２図は真空炉を示し、第３図に示す１０コイル
ヒーター１３を使用するものである。Further, FIG. 2 shows a vacuum furnace, in which a ten-coil heater 13 shown in FIG. 3 is used.
従来、マンドレル、アンカー、サポート、Ｍｏ箔などの
電球用に使用されているＭｏ材は常温における加工性と
経済性が主眼となっていた。しかしながら、ハロゲンラ
ンプの出現により一般照明、映写、光学及び自動車用電
球なども高効率、高寿命ランプと急転換している。この
ため、従来比較的低い温度（再結晶温度以下）で使用さ
れていたＭ。Conventionally, Mo materials used for light bulbs such as mandrels, anchors, supports, and Mo foils have focused on workability and economy at room temperature. However, with the advent of halogen lamps, general lighting, projection, optical, and automobile light bulbs are rapidly changing to high-efficiency, long-life lamps. For this reason, M has conventionally been used at relatively low temperatures (below the recrystallization temperature).
材についても耐高温特性にすぐれ、且つ高温度処理を施
し再結晶後も、従来のＭｏ材のように常温において脆化
しないで加工性のよいＭｏ材を得ることが課題となって
いる。また、ハロゲンランプ用ＭＯ部品以外の炉用ヒー
ターなどにおいても同様な特性を要求されている。It is also a challenge to obtain a Mo material that has excellent high-temperature resistance properties and has good workability without becoming brittle at room temperature like conventional Mo materials even after high-temperature treatment and recrystallization. Similar characteristics are also required for furnace heaters and the like other than MO parts for halogen lamps.
従って本発明の目的は、高温特性にすぐれ、且つ高温度
処理を施し再結晶後も常温下で脆化せず加工性にすぐれ
たＭｏ材を得る製造方法を提供することである。Therefore, an object of the present invention is to provide a manufacturing method for obtaining a Mo material that has excellent high-temperature properties, does not become brittle at room temperature even after recrystallization after high-temperature treatment, and has excellent workability.
本発明の第１は、＾Ｊ、Ｋ及びＳｔをＭＯ粉末にドープ
し且つＦｅ、 Ｎｉ、 Ｃｒを固溶させた粉末より成型
・焼結によって得られた焼結体の製造方法である。The first aspect of the present invention is a method for producing a sintered body obtained by molding and sintering a powder in which MO powder is doped with J, K, and St, and Fe, Ni, and Cr are dissolved in solid solution.
本発明の第２は第１の製造方法で得られたＭｏ棒、線材
を成型後又は成型前に２次再結晶処理をする方法である
。The second aspect of the present invention is a method in which the Mo rod or wire obtained by the first manufacturing method is subjected to a secondary recrystallization treatment after or before molding.
（１） 本発明の製造方法は、圧粉体を焼結して１４
Ｘ１４鶴の角柱棒状体を作製する。ついでここの工程に
おいて棒状全体に加工歪を与える。この場合５０％以下
の加工率では棒状体の加工歪が不均一となって、後工程
の熱処理において再結晶組織の周辺部のみが粗大結晶化
され以降の加工が不適当となる。また、８０％を越える
とスェージ加工中に割れが発生する頻度が多くなって歩
留を著しく悪化する。ついで、スェージ加工して得られ
た棒状体を再結晶温度より４００℃以上ないしは２００
０°Ｃ以下の温度で加熱処理することによって棒状体に
再結晶粒が生成する。再結晶粒の粒径は加えられる加工
歪及び加熱温度に存在される。即ち、加工歪が大きいほ
ど結晶粒はこまかくなる。(1) The manufacturing method of the present invention involves sintering a green compact and
A prismatic rod-shaped body of an X14 crane is prepared. Next, in this step, processing strain is applied to the entire rod shape. In this case, if the processing rate is less than 50%, the processing strain of the rod-like body will become non-uniform, and only the peripheral part of the recrystallized structure will be coarsely crystallized in the post-process heat treatment, making subsequent processing inappropriate. Moreover, if it exceeds 80%, cracks will occur more frequently during swaging, resulting in a significant decrease in yield. Then, the rod-shaped body obtained by swaging is heated to 400°C or more or 200°C higher than the recrystallization temperature.
Recrystallized grains are generated in the rod-shaped body by heat treatment at a temperature of 0°C or lower. The grain size of recrystallized grains depends on the applied processing strain and heating temperature. That is, the larger the processing strain, the finer the crystal grains.
このことによって加熱処理前に棒状体にスェージ加工し
て、棒状体に均一な歪を加えることにより再結晶粒が均
一となり、しかも再結晶温度より３００℃以上の温度に
加熱することにより２５〜４０μｍ程度のこまかい再結
晶粒が得られる。このＭｏ棒状体の再結晶温度は棒状体
に与えられる加工歪が大きいほど再結晶温度が低下する
。例えば、５０％の断面減少率では１５００℃程度であ
り、７０％の断面減少率では１３００℃程度まで低下す
る。このことにより同じ温度で加熱処理しても大きな加
工歪を加えた方が結晶粒は細かくなる。この場合、加熱
温度を上述した範囲に限定した理由は加熱処理温度が再
結晶温度より３００℃を越えない温度において再結晶し
た再結晶粒は大粒となって後工程で伸線加工を行なわれ
たときは、スェージ工程において割れを発生する。また
、加工歪が断面減少率８０％以上与えられるときは結晶
粒は微細になりすぎて伸線加工においてクラックが発生
し易くなる。また、２０００℃を越える温度では結晶粒
の微細効果が飽和状態に達する。By swaging the rod-shaped body before heat treatment and applying uniform strain to the rod-shaped body, the recrystallized grains become uniform, and by heating to a temperature of 300°C or more above the recrystallization temperature, the grain size becomes 25 to 40 μm. Fine recrystallized grains can be obtained. The recrystallization temperature of this Mo rod-like body decreases as the processing strain applied to the rod-like body increases. For example, at a reduction rate of 50%, the temperature decreases to about 1500°C, and at a reduction rate of 70%, the temperature decreases to about 1300°C. As a result, even if the heat treatment is carried out at the same temperature, the crystal grains become finer when a large processing strain is applied. In this case, the reason why the heating temperature was limited to the above-mentioned range is that when the heat treatment temperature does not exceed 300°C above the recrystallization temperature, the recrystallized grains become large and are subjected to wire drawing in the subsequent process. In some cases, cracks occur during the swaging process. Furthermore, when the processing strain is applied with a reduction in area of 80% or more, the crystal grains become too fine and cracks are likely to occur during wire drawing. Further, at temperatures exceeding 2000° C., the effect of fine crystal grains reaches a saturated state.
の線径のＭｏｖＡを製造する。A wire diameter of MovA is manufactured.
＋２１ ＋１）法で得られたＡＮ、に、Ｓｉ及びＦｅ
、 Ｎｉ。+21 +1) In the AN obtained by the method, Si and Fe
, Ni.
Ｃｒ含有のＭｏ材は通常は１０００〜１４００°Ｃ間で
の歪取り焼鈍を行って２次成形加工を施す。Cr-containing Mo material is usually subjected to strain relief annealing at 1000 to 1400°C and subjected to secondary forming processing.
（１）表１に７１１’ ＋ Ｓｔ ＋ Ｋ及びＦｅ、
Ｎｉ、 Ｍｏを含有した焼結体の分析値と試料磁を示
す。(1) Table 1 shows 711' + St + K and Fe,
The analytical values and sample magnets of a sintered body containing Ni and Mo are shown.
以下今日
表１
表１に示した各焼結体を１４００℃以下でスェージ加工
を行い、中間で熱処理を行い９７％以上のスェージ加工
及び伸線加工を行って各試料を作製した。Table 1 below: Each sintered body shown in Table 1 was swaged at 1400° C. or below, heat treated in the middle, and swaged and wire drawn to a rate of 97% or higher to produce each sample.
以下舎臼
（２） （１１項における表１１表２の試料Ｉｌ＆Ｌ
３によって作製された試料の線径０．８．０．６０．０
．３５ｆｉφに関する実施例を示す。Below is the mill (2) (Table 11 in Section 11 Table 2 Samples Il&L
Wire diameter of sample prepared by 3: 0.8.0.60.0
．． An example regarding 35fiφ will be shown.
試料隘３の焼結体を１４００℃以下でスェージ加工を行
い、スェージ加工の途中線径８．９ｆｉφにおいて１８
００℃の温度で熱処理を行い、以降スェージ及び線引加
工を行って所望の試験線径とし、１３００℃Ｘ２０分の
歪取り処理を行い試験片を作製した。The sintered body in sample chamber 3 was swaged at a temperature below 1400°C, and during the swaging process, the wire diameter was 8.9fiφ and 18
Heat treatment was performed at a temperature of 00°C, and thereafter swaging and wire drawing were performed to obtain a desired test wire diameter, and a strain relief treatment was performed at 1300°C for 20 minutes to prepare a test piece.
各線材の再結晶カーブを水素雰囲気中にて２０分間保持
した加熱処理温度と最大引張応力（δｕＴｓ ）の関係
において第４図に示す。第４図より粗大結晶化温度（臨
界点）は０．８ｆｉφ１４５０℃、０、６０ ＊＊φ１
５５０℃、０．３５ｍφ１６５０℃を示す。The recrystallization curve of each wire is shown in FIG. 4 in terms of the relationship between the heat treatment temperature maintained in a hydrogen atmosphere for 20 minutes and the maximum tensile stress (δuTs). From Figure 4, the coarse crystallization temperature (critical point) is 0.8fiφ1450℃, 0,60 **φ1
550℃, 0.35mφ1650℃.
第４図において、加熱処理温度０．８ ｗφ１５００℃
、０、６０ ｗφ１６００℃、０．３５ ＊ｓφ１７０
０℃の温度においてはδＵＴＳは約１００ｋｇ／ｗ”の
値が５０ｋｇ／龍２まで低下して以降安定値を示す。In Figure 4, the heat treatment temperature is 0.8wφ1500℃
,0,60 wφ1600℃, 0.35 *sφ170
At a temperature of 0° C., δUTS decreases from about 100 kg/w” to 50 kg/Ryu2 and then shows a stable value.
第５図は上述の各々の温度における加熱処理後の顕微鏡
組織を示す。第５図から明らかなように、粗大結晶下部
（０点）においては未だ繊維構造を維持しているがδａ
ｙｓが急降下したＴ点のそれはクサビ状にかみ合った数
層の線軸に平行な長大な結晶に変換している。FIG. 5 shows the microstructure after heat treatment at each of the above-mentioned temperatures. As is clear from Fig. 5, the fiber structure is still maintained in the lower part of the coarse crystals (point 0), but δa
The point at T, where ys suddenly falls, transforms into a long crystal parallel to the line axis of several interlocking layers in a wedge shape.
次に、加熱処理を施して最大結晶化した試片と処理前の
試片とをＪＩＳ ８４４６０−１９８４ ７項の加熱変
形試験法によ・って変形率を試験を行った結果を示す。Next, the results of testing the deformation rate of specimens that were subjected to heat treatment to achieve maximum crystallization and specimens before treatment using the heat deformation test method of JIS 84460-1984 Section 7 are shown.
第６図は加熱変形試験装置を示す。１１のようにヘアピ
ンに成形した試験片に所定のおもり１２をかけたまま、
露点−４０℃以下の水素ガス又はアンモニア分解ガスを
流したペルジャーの中で所定電流で一定時間通電加熱す
る。冷却後おもりを外して第６図のＳを測定した後試験
を行う。FIG. 6 shows a heating deformation test device. With a predetermined weight 12 applied to a test piece formed into a hairpin as shown in 11,
The sample is heated with a predetermined current for a predetermined period of time in a Pel jar in which hydrogen gas or ammonia decomposition gas having a dew point of -40° C. or lower is flowed. After cooling, remove the weight, measure S in Figure 6, and then conduct the test.
成形後、再び所定電流で一定時間通電加熱し、冷却後試
験片を取り外し、変形量を測定する。加熱温度はのぞき
窓より光高温計（パイロメーター）にて測定する。After molding, the test piece is heated again with a predetermined current for a certain period of time, and after cooling, the test piece is removed and the amount of deformation is measured. The heating temperature is measured using an optical pyrometer through the viewing window.
成形及び試験条件を表３に示す。Table 3 shows the molding and test conditions.
以下舎日 変形量測定方法及び評価方法について説明する。Below is the date A method for measuring the amount of deformation and an evaluation method will be explained.
ヘアピンは加熱後、第７図のように変形する。変形のＳ
＋ΔＳを目盛板などで読みとり （Ｓ＋ΔＳ）龍又は（
ΔＳ／Ｓｘ １００）％で表示する。After heating, the hairpin deforms as shown in Figure 7. S of transformation
Read +ΔS with a scale plate, etc. (S+ΔS) Dragon or (
Displayed as ΔS/Sx 100)%.
表４に実験結果を示す。Table 4 shows the experimental results.
表４に各試験片の加工方法及び熱処理以降の工程の加工
損率を示す。その結果、本発明の方法においては加工の
損率が２％以下となるが、比較用の方法ではいずれも加
工損率が悪い。特に熱処理なしの１ＩｋＬ１０は９０％
以上の損率である。この損率は線材のクラック欠陥であ
る。Table 4 shows the processing method of each test piece and the processing loss rate of the steps after heat treatment. As a result, in the method of the present invention, the machining loss rate is 2% or less, but in all the comparative methods, the machining loss rate is poor. Especially 1IkL10 without heat treatment is 90%
This is the loss ratio. This loss factor is a crack defect in the wire.
以下今日 第 ４ 表 以下宗日Below today Table 4 Souichi below
第１図はＭｏ材の使用されるＪＩＳＨＡタイプのハロゲ
ンランプの模式図、
第２図は真空炉を示す側断面図、
第３図は第２図の真空炉に用いられるコイルヒータを示
す側面図、
第４図は試料光３から得た３種の線径の線材の加熱処理
温度と最大引張応力との関係図、第５図は第４図で示す
３種の線材の加熱処理後の顕微鏡組織図、
第６図は加熱変形試験装置を示す側面図、第７図は加熱
変形量測定により変形したヘアピンを示す図である。
１・・・石英ガラス又は硬質ガラス、２・・・Ｗフィラ
メント、３・・・Ｍｏミラー、４・・・Ｗフィラメント
、５・・・Ｍｏサポート、６・・・財スリーブ、７・・
・Ｍｏサポート、８・・・Ｍｏ箔、９・・・Ｆｅ−Ｎｉ
リード線、１０・・・封入部、１１・・・試験片、１２
・・・おもり、１３・・・コイルヒータ。
第１図
第２図
第４図
第５図Figure 1 is a schematic diagram of a JISHA type halogen lamp using Mo material, Figure 2 is a side sectional view showing a vacuum furnace, and Figure 3 is a side view showing a coil heater used in the vacuum furnace shown in Figure 2. , Figure 4 is a diagram of the relationship between heat treatment temperature and maximum tensile stress for wire rods of three diameters obtained from sample light 3, and Figure 5 is a microscope view of the three types of wire rods shown in Figure 4 after heat treatment. FIG. 6 is a side view showing the heating deformation testing device, and FIG. 7 is a diagram showing the hairpin deformed by measuring the amount of heating deformation. DESCRIPTION OF SYMBOLS 1... Quartz glass or hard glass, 2... W filament, 3... Mo mirror, 4... W filament, 5... Mo support, 6... Material sleeve, 7...
・Mo support, 8...Mo foil, 9...Fe-Ni
Lead wire, 10...Enclosed part, 11...Test piece, 12
...Weight, 13...Coil heater. Figure 1 Figure 2 Figure 4 Figure 5
Claims (1)
、Ｃｒ元素を固溶化させて焼結体を得、スエージ又は溝
ロール加工工程において焼結体からの断面減少率が５０
〜８０％となるように、棒状体の再結晶温度である４０
０℃以上、２０００℃以下の温度で加熱処理を行うとと
もに、更にそれ以降のスエージ及び線引加工を９７％以
上行うことを特徴とするモリブデン材の製造方法。 ２、前記モリブデン材から製造される線材又は棒材を粗
大結晶化温度より１００℃以上高い温度で加熱処理を行
う特許請求の範囲第１項記載の製造方法。[Claims] 1. Fe, Ni in the presence of Al, K, Si dopants
, a sintered body is obtained by solid solutioning the Cr element, and the area reduction rate from the sintered body is 50 in the swaging or groove rolling process.
40, which is the recrystallization temperature of the rod, so that the
A method for producing a molybdenum material, which comprises performing heat treatment at a temperature of 0° C. or higher and 2000° C. or lower, and further performing 97% or more of swaging and wire drawing. 2. The manufacturing method according to claim 1, wherein the wire rod or rod manufactured from the molybdenum material is heat-treated at a temperature 100° C. or more higher than the coarse crystallization temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31132286A JPS63166952A (en) | 1986-12-27 | 1986-12-27 | Manufacture of molybdenum material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP31132286A JPS63166952A (en) | 1986-12-27 | 1986-12-27 | Manufacture of molybdenum material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63166952A true JPS63166952A (en) | 1988-07-11 |
| JPH0129863B2 JPH0129863B2 (en) | 1989-06-14 |
Family
ID=18015740
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP31132286A Granted JPS63166952A (en) | 1986-12-27 | 1986-12-27 | Manufacture of molybdenum material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63166952A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017151737A1 (en) * | 2016-03-03 | 2017-09-08 | H.C. Starck Inc. | Fabricaton of metallic parts by additive manufacturing |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59150071A (en) * | 1983-02-10 | 1984-08-28 | Toshiba Corp | Production of molybdenum material |
| JPS6127459A (en) * | 1984-07-17 | 1986-02-06 | 松下電器産業株式会社 | Refrigeration cycle device for multi-chamber corresponding type air conditioner |
-
1986
- 1986-12-27 JP JP31132286A patent/JPS63166952A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59150071A (en) * | 1983-02-10 | 1984-08-28 | Toshiba Corp | Production of molybdenum material |
| JPS6127459A (en) * | 1984-07-17 | 1986-02-06 | 松下電器産業株式会社 | Refrigeration cycle device for multi-chamber corresponding type air conditioner |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017151737A1 (en) * | 2016-03-03 | 2017-09-08 | H.C. Starck Inc. | Fabricaton of metallic parts by additive manufacturing |
| US10099267B2 (en) | 2016-03-03 | 2018-10-16 | H.C. Starck Inc. | High-density, crack-free metallic parts |
| US10730089B2 (en) | 2016-03-03 | 2020-08-04 | H.C. Starck Inc. | Fabrication of metallic parts by additive manufacturing |
| US10926311B2 (en) | 2016-03-03 | 2021-02-23 | H.C. Starck Inc. | High-density, crack-free metallic parts |
| US11458519B2 (en) | 2016-03-03 | 2022-10-04 | H.C. Stark Solutions Coldwater, LLC | High-density, crack-free metallic parts |
| US11554397B2 (en) | 2016-03-03 | 2023-01-17 | H.C. Starck Solutions Coldwater LLC | Fabrication of metallic parts by additive manufacturing |
| US11826822B2 (en) | 2016-03-03 | 2023-11-28 | H.C. Starck Solutions Coldwater LLC | High-density, crack-free metallic parts |
| US11919070B2 (en) | 2016-03-03 | 2024-03-05 | H.C. Starck Solutions Coldwater, LLC | Fabrication of metallic parts by additive manufacturing |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0129863B2 (en) | 1989-06-14 |
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