JP2005111562A - Method for cold-deformation processing of molybdenum using backward extrusion - Google Patents

Method for cold-deformation processing of molybdenum using backward extrusion Download PDF

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JP2005111562A
JP2005111562A JP2004270451A JP2004270451A JP2005111562A JP 2005111562 A JP2005111562 A JP 2005111562A JP 2004270451 A JP2004270451 A JP 2004270451A JP 2004270451 A JP2004270451 A JP 2004270451A JP 2005111562 A JP2005111562 A JP 2005111562A
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molybdenum
cold
backward extrusion
under vacuum
recrystallization
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JP4348266B2 (en
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Bernd Spaniol
シュパニオール ベルント
Josef Trageser
トラゲザー ヨーゼフ
Wolfgang Guenther
ギュンター ヴォルフガング
Joerg Schielke
シールケ イェルク
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WC Heraus GmbH and Co KG
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22FCHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/16Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18High-melting or refractory metals or alloys based thereon
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/002Extruding materials of special alloys so far as the composition of the alloy requires or permits special extruding methods of sequences
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B21MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21CMANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C23/00Extruding metal; Impact extrusion
    • B21C23/02Making uncoated products
    • B21C23/18Making uncoated products by impact extrusion
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01JELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02Manufacture of electrodes or electrode systems
    • H01J9/022Manufacture of electrodes or electrode systems of cold cathodes

Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing a molybdenum molding member without a crack nor a break by cold-deformation processing using backward extrusion. <P>SOLUTION: A molybdenum work piece is completely recrystallized at a temperature exceeding 1,400 degree C under vacuum and/or under protection gas and is cooled under vacuum and/or under protection gas. Then, the molybdenum work piece is subjected to the cold-deformation processing using backward extrusion at room temperature. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

本発明は、モリブデンを後方押出しによって冷間変形加工するための方法に関する。   The present invention relates to a method for cold deformation of molybdenum by backward extrusion.

モリブデンはその熱的な特性、電気的な特性および化学的な特性のため照明工学に使用される。モリブデンは室温で脆弱性の材料であり、前製品および半製品は一般的に熱間で変形加工される。モリブデン成形部材、たとえば照明工学に用いられる管またはキャップは、板材および帯材から室温で深絞り加工によって製作することができる。深絞り加工とは、板材から中空体への引張り・圧縮変形加工(Zugdruckumformen)または大きな外周の中空体からのより小さな外周を備えた中空体の成形を意味している。この場合、板材厚さは故意に変えられない。切断された板材が収容部内に置かれる。押さえが板材を絞りダイに向かって押圧し、これによって、深絞りの間に皺(しわ)形成を阻止する。下降する絞りラムが板材を絞りダイ内に押圧し、これによって、板材を所望のワークに成形する。絞り比が高い場合には、深絞り加工が多くのステップで実施され得る。絞り比とは、ワークの直径に対する、切断された板材の直径の比率を意味している。深絞り加工ステップの間に中間焼鈍しが行われ得る。   Molybdenum is used in lighting engineering due to its thermal, electrical and chemical properties. Molybdenum is a brittle material at room temperature, and the previous and semi-finished products are generally deformed hot. Molybdenum molded parts, such as tubes or caps used in lighting engineering, can be made from plate and strip by deep drawing at room temperature. Deep drawing means tension / compression deformation (Zugdruckumformen) from a plate material to a hollow body or molding of a hollow body with a smaller outer periphery from a large outer peripheral hollow body. In this case, the plate thickness cannot be changed intentionally. The cut | disconnected board | plate material is set | placed in an accommodating part. The presser presses the plate material toward the drawing die, thereby preventing wrinkle formation during deep drawing. The squeezing ram that descends presses the plate into the drawing die, thereby forming the plate into a desired workpiece. If the drawing ratio is high, deep drawing can be performed in many steps. The drawing ratio means the ratio of the diameter of the cut plate material to the diameter of the workpiece. Intermediate annealing may be performed during the deep drawing step.

前製品および半製品の変形加工は一般的に熱間で、すなわち、有利には焼結直後に(アメリカ合衆国特許第5158709号明細書参照)(または電子ビーム溶解されたモリブデンでは熱間鍛造後に)または熱機械的な変形加工によって行われる(アメリカ合衆国特許第5051139号明細書参照)。有利には細い寸法の場合の冷間の変形加工法も存在している。しかし、この場合、モリブデンは、加工時に引張り応力下で亀裂または破断が生ぜしめられないように完全に再結晶化されない。慣用の教義は、材料が完全に再結晶化されてはならないと言っている。なぜならば、この場合、再結晶化された軟焼鈍しされた状態で、変形加工のために必要となる引張り応力が材料の破壊(収縮、亀裂)を生ぜしめる恐れがあるからである。   Deformation of the previous product and the semi-finished product is generally hot, ie preferably immediately after sintering (see US Pat. No. 5,158,709) (or after hot forging in electron beam melted molybdenum) or This is performed by thermomechanical deformation (see US Pat. No. 5,051,139). There are also advantageously cold deformation methods for small dimensions. In this case, however, the molybdenum is not completely recrystallized so that cracks or breaks do not occur under tensile stress during processing. Conventional doctrine says that the material must not be completely recrystallized. This is because, in this case, the tensile stress necessary for deformation processing may cause destruction (shrinkage or cracking) of the material in the recrystallized soft annealed state.

さらに、変形加工、再結晶化および熱処理が交互に行われる方法が公知である(たとえばアメリカ合衆国特許第4600446号明細書参照)。   Further, a method in which deformation processing, recrystallization and heat treatment are alternately performed is known (see, for example, US Pat. No. 4,600,466).

押出し加工による、再結晶化されたかもしくは応力除去された脆弱性の材料(これにはモリブデンが属している)の冷間変形加工のための方法は、アメリカ合衆国特許第3552996号明細書に記載されている。この方法は前方押出しとしても公知である。押出し加工とは、中空体または中実体を製作するための冷間変形加工法である。コンパクトな前材料(ビレット)が、押出し成形に類似して、ラムによってダイを通して(前方に)プレスされるかまたはラムが前材料内にプレスされ、材料がラムに沿って後方に流れる。押出し成形に対する違いは処理温度および押出し加工によって半製品ストランドではなく、個別部材が製作されることにある。この場合、複雑な形も製作することができる。方法の利点は、少ない金型コスト、高い金型寿命および約30〜150個/分のサイクル時間を備えた高い作業速度にある。表面品質は良好であり、後続の表面処理のために適している。主使用分野はアルミニウム合金である。主着眼点は、アメリカ合衆国特許第3552996号明細書に記載された方法では、押出しダイにおける険しい引裂き縁部の回避にある。これによって、変形加工後の急激な応力移行が回避されるようになっている。しかし、前述した方法は、TZM合金に対してしか実際に確保されておらず、これによって、いずれにせよ、部分的に亀裂なしの成形体を形成することができる(例参照)。
アメリカ合衆国特許第5158709号明細書 アメリカ合衆国特許第5051139号明細書 アメリカ合衆国特許第4600446号明細書 アメリカ合衆国特許第3552996号明細書
A method for cold deformation processing of recrystallized or stress relieved brittle materials (to which molybdenum belongs) by extrusion is described in US Pat. No. 3,552,996. Yes. This method is also known as forward extrusion. Extrusion is a cold deformation method for producing a hollow body or solid body. A compact pre-material (billet) is pressed through the die ( forward ) by the ram, similar to extrusion, or the ram is pressed into the pre-material and the material flows backward along the ram. The difference to extrusion is that individual parts are produced, not semi-finished strands, by processing temperature and extrusion. In this case, complex shapes can also be produced. The advantage of the method is high working speed with low mold cost, high mold life and cycle time of about 30-150 pieces / min. The surface quality is good and suitable for subsequent surface treatment. The main field of use is aluminum alloys. The main focus is in the avoidance of steep tear edges in the extrusion die in the method described in US Pat. No. 3,552,996. This avoids abrupt stress transition after deformation. However, the above-described method is only actually ensured for TZM alloys, and in this way, a partially crack-free molded body can be formed anyway (see the example).
United States Patent No. 5,158,709 US Pat. No. 5,051,139 United States Patent No. 4,600,466 US Pat. No. 3,552,996

したがって、本発明の課題は、冒頭で述べた形式の、モリブデンを後方押出しによって冷間変形加工するための方法を改良して、亀裂または破断なしの成形部材を製作することができるようにする。   The object of the present invention is therefore to improve the method for cold deformation of molybdenum by backward extrusion of the type mentioned at the outset so that molded parts without cracks or breaks can be produced.

この課題を解決するために本発明の方法では、冷間変形加工前に完全な再結晶化を実施するようにした。   In order to solve this problem, in the method of the present invention, complete recrystallization is performed before cold deformation.

いま、本発明では、モリブデンを後方押出しによって冷間変形加工するための方法が記載される。モリブデンは、驚くべきことに、その脆弱性にもかかわらず、亀裂または破断が生ぜしめられることなしに、後方押出しによって変形加工することができることが分かった。押出し加工時には、エネルギが押圧応力によって加えられる。モリブデンは、十分に僅かな応力で材料の降伏点を上回らないために、予め熱処理によって完全に再結晶化される。再結晶化時には、予め変形加工によって生ぜしめられた全てのグリッド応力が除去されることが望ましい。この場合、材料は比較的僅かな力でその降伏点に到達する。再結晶化は、有利には1300℃、特に1400℃を上回る温度で行われる(モリブデンの融点は2623〜5℃にある)。   Now, in the present invention, a method for cold deformation of molybdenum by backward extrusion is described. It has been surprisingly found that molybdenum, despite its fragility, can be deformed by backward extrusion without causing cracks or breaks. At the time of extrusion, energy is applied by pressing stress. Molybdenum is completely recrystallized by heat treatment in advance so that it does not exceed the yield point of the material with sufficiently little stress. At the time of recrystallization, it is desirable to remove all grid stress previously generated by deformation processing. In this case, the material reaches its yield point with relatively little force. The recrystallization is preferably carried out at temperatures above 1300 ° C., in particular above 1400 ° C. (molybdenum has a melting point of 2623-5 ° C.).

したがって、本発明は、モリブデンを後方押出しによって冷間変形加工するための方法に関する。この場合、予め完全な再結晶化が実施される。方法は、有利には以下の通り実施される。   The present invention therefore relates to a method for cold deformation of molybdenum by backward extrusion. In this case, complete recrystallization is performed in advance. The method is advantageously carried out as follows.

のちの完成品の直径範囲におけるモリブデン線材が、真空下でまたは保護ガス下で1400℃を上回る温度で完全に再結晶化され、真空下でまたは保護ガス下で冷却される。こうして再結晶化された材料から成る区分が室温で押出し加工されて、回転対称的な完成品が形成される。   Later the molybdenum wire in the diameter range of the finished product is completely recrystallized at a temperature above 1400 ° C. under vacuum or under protective gas and cooled under vacuum or under protective gas. The sections of recrystallized material are extruded at room temperature to form a rotationally symmetric finished product.

方法の主要な利点:第1には、材料を深絞り加工の場合よりも著しく良好に使用することができる。さらに、より肉厚なまたは成形された底部を備えた部材を後方押出しによって製作することができる。方法は、別の脆弱性の金属またはその合金、たとえばクロムまたはタングステンのためにも適している。   Major advantages of the method: First, the material can be used significantly better than in deep drawing. Furthermore, a member with a thicker or molded bottom can be produced by backward extrusion. The method is also suitable for other brittle metals or their alloys, such as chromium or tungsten.

産業的には、方法は、たとえば照明工学に用いられるモリブデンキャップを製作するために使用することができる。こうして製作された部材は、CCFL(Cold Cathode Fluorescent Lighting)ランプもしくは冷陰極ランプ(KKL)におけるガラスバルブまたはセラミックスバルブを貫く電流案内部およびエミッタ電極として使用することができる。冷陰極ランプもしくはCCFLランプは蛍光灯であり、低圧放電の原理を使用している。これによって、希薄のガス混合物が励起される(たとえばAr/Hg)。電極は加熱されず、まず、高い電圧が管に印加され、これによって、ガス混合物がイオン化され、導電性にされる。電気的なエネルギがガス原子を励起し、過剰のエネルギをUV光および可視光の形で再び放出する。管の内面に設けられた燐ベースの被覆層はUV放射線を可視光に変換する。電極は高融点金属、たいていモリブデンから製作される。このモリブデンは、特に容易に電子を放出するという特性のため適している。交流運転時には、電極が交互に陰極および陽極として機能する。   Industrially, the method can be used to fabricate molybdenum caps used, for example, in lighting engineering. The member thus manufactured can be used as a current guide and an emitter electrode that penetrates a glass bulb or a ceramic bulb in a CCFL (Cold Cathode Fluorescent Lighting) lamp or a cold cathode lamp (KKL). Cold cathode lamps or CCFL lamps are fluorescent lamps and use the principle of low pressure discharge. This excites a lean gas mixture (eg, Ar / Hg). The electrodes are not heated and a high voltage is first applied to the tube, which ionizes the gas mixture and makes it conductive. Electrical energy excites gas atoms and releases excess energy again in the form of UV and visible light. A phosphorus-based coating layer provided on the inner surface of the tube converts UV radiation into visible light. The electrodes are made from a refractory metal, usually molybdenum. Molybdenum is particularly suitable because of its property of easily releasing electrons. During AC operation, the electrodes function alternately as a cathode and an anode.

以下に、本発明を実施するための最良の形態を図面につき詳しく説明する。   In the following, the best mode for carrying out the invention will be described in detail with reference to the drawings.

1400℃よりも高い温度で真空下で再結晶化された、真空下で冷却された1mmのモリブデン線材区分から、約1500MPaの圧力下で室温でプレスにおいて、成形されるキャップが後方に押出し加工される。   From a 1 mm molybdenum wire segment recrystallized under vacuum at a temperature higher than 1400 ° C. and cooled under vacuum, the molded cap is extruded backwards in a press at room temperature under a pressure of about 1500 MPa. The

このようなキャップは、エミッタ電極としてCCFL(冷陰極管)ランプに使用することができる。   Such a cap can be used for a CCFL (cold cathode tube) lamp as an emitter electrode.

説明した方法により、使用される材料が廃物なしに100%変形加工される。   By the method described, the material used is deformed 100% without waste.

この方法により製作された、図1に示したキャップの顕微鏡レベルの縦断面は、この方法で亀裂なしの回転対称的な成形部材を製作することができることを示している。   The microscopic level cross section of the cap shown in FIG. 1 produced by this method shows that a rotationally symmetric molded member without cracks can be produced by this method.

本発明による方法により製作されたモリブデンキャップの縦断面を50:1の縮尺で示す図である。FIG. 3 shows a longitudinal section of a molybdenum cap made by the method according to the invention on a 50: 1 scale.

Claims (7)

モリブデンを後方押出しによって冷間変形加工するための方法において、冷間変形加工前に完全な再結晶化を実施することを特徴とする、モリブデンを後方押出しによって冷間変形加工するための方法。   A method for cold deformation of molybdenum by backward extrusion, characterized in that complete recrystallization is performed before cold deformation in a method for cold deformation of molybdenum by backward extrusion. 再結晶化を保護ガス下でかつ/または真空下で実施する、請求項1記載の方法。   The process according to claim 1, wherein the recrystallization is carried out under protective gas and / or under vacuum. 再結晶化を1300℃を上回る温度で実施する、請求項1または2記載の方法。   The process according to claim 1 or 2, wherein the recrystallization is carried out at a temperature above 1300 ° C. A)モリブデンワークを真空下でかつ/または保護ガス下で1400℃を上回る温度で完全に再結晶化し、
B)ワークを真空下でかつ/または保護ガス下で冷却し、
C)こうして再結晶化されたワークから成る区分を室温で押出し加工して、完成品を形成する、請求項1から3までのいずれか1項記載の方法。
A) completely recrystallizing the molybdenum workpiece under vacuum and / or under protective gas at a temperature above 1400 ° C.
B) cooling the workpiece under vacuum and / or under protective gas,
4. A method according to claim 1, wherein the section comprising the workpiece thus recrystallized is extruded at room temperature to form a finished product.
完成品を回転対称的にプレス加工する、請求項4記載の方法。   5. A method according to claim 4, wherein the finished product is pressed rotationally symmetrically. 当該方法により押出し加工されたモリブデン成形部材を照明工学に使用する、請求項1から5までのいずれか1項記載の方法。   The method according to claim 1, wherein the molybdenum molded member extruded by the method is used for lighting engineering. 当該方法を、CCFLランプもしくは冷陰極ランプにおけるガラスバルブまたはセラミックスバルブを貫く電流案内部の製作またはエミッタ電極の製作のために使用する、請求項6記載の方法。   7. The method according to claim 6, wherein the method is used for the production of current guides or emitter electrodes through glass or ceramic bulbs in CCFL lamps or cold cathode lamps.
JP2004270451A 2003-10-02 2004-09-16 Method for cold deformation of molybdenum by backward extrusion Expired - Fee Related JP4348266B2 (en)

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