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WO2015064808A1 - Procédé de fabrication d'alliage platine-rhodium renforcé par dispersion d'oxyde pour la fabrication de verre à cristaux liquides par utilisation d'un frittage par plasma d'étincelles - Google Patents

Procédé de fabrication d'alliage platine-rhodium renforcé par dispersion d'oxyde pour la fabrication de verre à cristaux liquides par utilisation d'un frittage par plasma d'étincelles Download PDF

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Publication number
WO2015064808A1
WO2015064808A1 PCT/KR2013/009983 KR2013009983W WO2015064808A1 WO 2015064808 A1 WO2015064808 A1 WO 2015064808A1 KR 2013009983 W KR2013009983 W KR 2013009983W WO 2015064808 A1 WO2015064808 A1 WO 2015064808A1
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Prior art keywords
platinum
rhodium
oxide
alloy
manufacturing
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Ceased
Application number
PCT/KR2013/009983
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English (en)
Korean (ko)
Inventor
윤원규
양승호
박재성
연병훈
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
LT Metal Co Ltd
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Heesung Metal Ltd
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Filing date
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Publication of WO2015064808A1 publication Critical patent/WO2015064808A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0466—Alloys based on noble metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
    • B22F3/10—Sintering only
    • B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
    • B22F2003/1051—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding by electric discharge
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2201/00—Treatment under specific atmosphere
    • B22F2201/50—Treatment under specific atmosphere air
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
    • B22F2998/10—Processes characterised by the sequence of their steps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy

Definitions

  • the present invention enhances the dispersion of high-density oxides used as platinum devices (melting devices, crucibles, bushings, stirrers) in LCD glass manufacturing industries due to their high melting point and high temperature strength. It relates to a method of manufacturing a type platinum-rhodium alloy, and more particularly, to prepare a thin plate of the oxide dispersion-enhanced platinum-rhodium alloy using melt spinning method, and then heat treatment, discharge plasma sintering (SPS), forging, The present invention relates to a novel production method for producing a high density oxide dispersion-enhanced platinum-rhodium alloy material through post-processing such as rolling.
  • SPS discharge plasma sintering
  • Platinum which has high melting point, chemical resistance and corrosion resistance, is easy to process at room temperature and high temperature, and has excellent volatility, and thus has been used in various industries despite being an expensive material.
  • the use of platinum materials having excellent strength has been increasing for the manufacture of materials and devices for manufacturing high quality glass for LCDs.
  • the conventionally designed oxide dispersion-strengthened platinum-rhodium alloy is prepared by producing a platinum-rhodium alloy powder using plasma or melt spinning, and then secured by hot sintering, followed by hot working (forging and rolling). And the final heat treatment to obtain an oxide dispersion strengthened platinum-rhodium alloy plate.
  • the pressure sintering process such as hot press that is carried out in the process has a disadvantage that the cost is high due to the increase in the process time. There is a need for a new manufacturing method that shortens the process time and reduces the manufacturing cost.
  • the present invention has been made to solve the above-described problems, in the production of a platinum-rhodium alloy dispersed in an oxide having excellent high temperature strength and kryptok, after manufacturing a metal sheet by using melt spinning (Melt Spinning) Manufactured
  • the purpose of the present invention is to manufacture a high density oxide dispersion-enhanced platinum-rhodium alloy by manufacturing a high density oxide dispersion-enhanced platinum-rhodium alloy through discharge plasma sintering (SPS). It is done.
  • SPS discharge plasma sintering
  • the present invention comprises the steps of (a) adding an alloying element for rhodium and oxide of the desired composition to platinum to produce an alloy ingot for platinum-rhodium-oxide; (b) preparing a platinum-rhodium alloy thin plate by using a melt spinning method on the prepared platinum-rhodium-oxide alloy ingot; (c) subjecting the prepared platinum-rhodium alloy sheet to an oxidative heat treatment to oxidize an alloy element for oxide; (d) stacking or pulverizing the oxidized heat treated thin plate to improve density by discharge plasma sintering (SPS); And (e) provides a method for producing a platinum-rhodium alloy for the oxide dispersion strengthening for producing LCD Glass comprising the step of post-processing the sintered body.
  • SPS discharge plasma sintering
  • the step (b) is charged with a platinum-rhodium alloy ingot (melt) in the melt spinning equipment and melted, and then rotating the melt at a constant speed by pressure injection of argon gas through a nozzle
  • the metal sheet may be manufactured by contacting and entangling with a wheel surface.
  • the step (d) may be a high-temperature press-molding by spark plasma sintering (SPS) method, wherein 5 to 20 at a temperature of 1200 ° C to 1400 ° C It is preferably carried out under pressure conditions of 10 MPa to 50 MPa for minutes.
  • the post-processing step of step (e) is preferably carried out one or more processes selected from the group consisting of hot working, hot working and recrystallization heat treatment of the sintered body.
  • the discharge plasma sintering method SPS
  • the hot press sintering method is equivalent to a short time.
  • high density oxide dispersed hardened platinum-plated alloy plates be manufactured, but the process time and cost can be significantly reduced.
  • FIG. 1 is a process flowchart of a method for preparing an oxide dispersion strengthened platinum-rhodium alloy according to an embodiment of the present invention.
  • Figure 2 is a process flow chart comparing the conventional method and the oxide dispersion strengthening platinum-rhodium alloy production method according to the present invention.
  • Figure 3 is a graph showing the relative density value of the oxide dispersion-enhanced platinum-rhodium alloy and the process prepared in Comparative Example (conventional method) and Example, respectively.
  • FIG. 5 is a TEM analysis photograph of the oxide dispersion-enhanced platinum-rhodium alloy sheet prepared in Example.
  • 6 is an analysis photograph showing the grain size of the oxide dispersion-enhanced platinum-rhodium alloy prepared according to the present invention (Example-6b) and the conventional method (Comparative Example-6a).
  • Figure 7 is a graph showing the high temperature (800 ° C) tensile strength results of the oxide dispersion strengthened platinum-rhodium alloy prepared in accordance with the present invention (Example-7b) and the conventional method (Comparative Example-7a).
  • the present invention is characterized by producing a high-density oxide dispersion-enhanced platinum-rhodium alloy plate material of a similar level in a short time by replacing the conventional hot press with hot discharge sintering (SPS).
  • SPS hot discharge sintering
  • Spark plasma sintering is a method of sintering by applying a DC pils current in a direction parallel to the pressing direction while pressing powder or plate in one axis. It is a sintering method that applies high energy of plasma generated instantly by sparks generated at this time to electric field diffusion, thermal diffusion and the like.
  • the discharge plasma sintering method has a high power consumption since the sintering temperature is 200 to 50 (C lower than that of the conventional hot press method and the sintering can be completed in a short time including the temperature raising and holding time). Reduced, easy to handle, and low running cost.
  • the alloying elements in the internal oxidation process can be performed in a short time.
  • the prepared platinum alloy sheet is subjected to oxidation heat treatment and discharge plasma. After sintering, it can be produced by the post-processing method.
  • the manufacturing method will be described by dividing each step as follows.
  • an ingot of a platinum-rhodium-oxide alloy is prepared by adding a rhodium and an oxide reinforcing element having a desired composition to high purity platinum (S10).
  • the first step is to produce an element alloy ingot for platinum-rhodium-oxide in a vacuum or inert atmosphere.
  • the rhodium content in the alloying elements to be added may be appropriately controlled within the conventional range known in the art, and may be, for example, in the range of 5 to 20% by weight based on the total 100% by weight. Can be. At this time, if the rhodium content is less than 5% by weight, it is impossible to obtain a solid solution strengthening effect of rhodium. If the rhodium content is more than 20 wt%, the strength is increased and cracks are generated during post-processing. There is a disadvantage that the improvement is rather deteriorated.
  • the one or more metal elements added as the alloying element for the oxide may use any conventional metal component in the art used in the conventional platinum alloy without limitation.
  • the alloying element can be added in a variety of types, and does not impair corrosion resistance in consideration of the use in the glass industry, and has a higher oxidation degree than platinum and gold,
  • the alloy element for oxide that can be used include zirconium (Zr), samarium (Sm), yttrium (Y), hafnium (Hf), or one or more mixed forms.
  • the amount of the alloying element for the oxide is not particularly limited, but is preferably in the range 0.02% by weight to 0.8% by weight 0 /.
  • the content of the alloying elements for the oxide, and a dispersion strengthening effect is less than 0.02 0/0 negligible 0.8 Increased 0 / if it exceeds 0, the creep strength, but improved, and the dispersion strengthening effect due to the residual dispersed particles increases workability is lowered There is a disadvantage. Therefore, the amount of the alloy element for rhodium and oxide is preferably selected within the range capable of workability while maximizing the solid solution strengthening and dispersion strengthening effect.
  • the above-described oxide alloy element is more oxidative than platinum or rhodium, and when dissolved in air, it is difficult to control the content of the oxide element by oxidation and vaporization. Do.
  • the alloy ingot for platinum-rhodium-oxide is prepared into a thin metal sheet by using melt spinning.
  • the platinum-rhodium alloy ingot prepared by vacuum dissolution is charged into a melt spinning equipment and melted, and then argon gas through a nozzle
  • the molten metal may be manufactured by flowing the melt by contact with a wheel surface that rotates at a constant speed by pressurized injection of the melt.
  • the ingot is charged and the charged ingot is melted under high vacuum (KT 4 Torr) conditions.
  • a platinum alloy sheet is produced by pressing and argon gas (Ar Gas) from the nozzle on the surface of the rotating wheel (for example, Cu Wheel) rotating at a constant speed.
  • the rotational speed of the rotary wheel is not particularly limited, but may be in the range of 500 to 3000 rpm, for example.
  • the pressure injection range of the argon gas may be in the range of 0.1 to 1.0 MPa, but is not particularly limited thereto.
  • a material having a high melting point may be used without limitation, and preferably, a quartz crucible or a mold of graphite material is used.
  • the size and thickness of the metal sheet produced in the step can be adjusted according to the wheel speed, injection pressure, distance to the nozzle and the like.
  • the platinum-rhodium alloy thin plate may have a width in a range of about 3 to 10 mm, a thickness of 100 m or less, and preferably in a range of 5 to 100 mm.
  • Oxide heat treatment is performed on the produced platinum thin plate to produce a thin plate on which the element for oxide is oxidized (S30).
  • the oxide is formed and dispersed in a short time.
  • the heat treatment conditions are not particularly limited, but are preferably carried out at a temperature of 800 ° C to 1200 ° C and for 1 to 12 hours.
  • the heat treatment temperature is less than 800 ° C or less than 1 hour, the oxidation of the alloying element for the oxide may not be sufficient, and if the temperature exceeds 1200 ° C, 12 hours, the dispersion strengthening effect by the interaction of the oxide of the alloying element There is a disadvantage that is lowered.
  • the shape to be manufactured is a thin plate, it is preferable to produce a thin plate shape so that the oxidation of the alloying element which is easy to oxidize in a short time can be sufficiently performed.
  • the discharge plasma sintering method is performed instead of the hot press sintering method (hot press) to ensure high density of the sintered body.
  • the discharge plasma sintering method refers to the sintering of high energy of a high-temperature discharge plasma instantaneously generated by spark discharge by the action of thermal diffusion, electric field diffusion, and the like.
  • a sintering process such as HIP (hot isostatic press)
  • HIP hot isostatic press
  • platinum alloy foil which is an oxidized molded body After laminating or pulverizing the plate and inserting it into the mold, the powder material is subjected to pressure, direct current pulse electrical energy, and large current, so that the high energy of the discharge plasma generated instantaneously by the discharge phenomenon between powder particles can be obtained. It is intended to have a target density through discharge plasma sintering (SPS), which is effectively sintered by thermal diffusion and electric field diffusion.
  • SPS discharge plasma sintering
  • the applicable sintering conditions are preferably carried out at a pressure of 10 to 50 MPa for 5 to 20 minutes in the temperature range of 1200 ° C to 1400 ° C.
  • the sintering temperature is less than 120 (C or low sintering time and pressure can not be obtained high density sintered body, if the temperature is more than 1400 ° C, sintering time is more than 20 minutes, the characteristics due to coarsening of the acid deteriorate Higher pressures are also undesirable, as high pressures can pose a hazard to the application molds and equipment.
  • the target density range of the sintered body produced by the sintering method may have a range of about 80 to 90%.
  • the sintered body produced by the discharge plasma sintering method (SPS) of the present invention is about 86.2% even if it is sintered at a relatively low temperature for a short time This can represent the relative density of.
  • An oxide dispersion-reinforced platinum-rhodium alloy material is finally produced by post-processing the sintered body produced by the discharge plasma sintering method (S50).
  • the post-processing may be to perform one or more processes selected from the group consisting of hot working, hot working and recrystallization heat treatment of the sintered body.
  • hot working, cold working and recrystallization heat treatment are performed sequentially.
  • the hot working process is important to ensure the density close to the theoretical density.
  • non-limiting examples of the applicable hot working process is hot rolling, it is possible to use a hot forging process.
  • the processing temperature during the hot working can be appropriately adjusted in the conventional range known in the art, for example, it is preferably carried out in the range of 1,000 ⁇ 1400 ° C. If the processing temperature is less than 1000 ° C, cracks are likely to occur during hot working, it is difficult to ensure high density, and if it exceeds 1400 ° C, oxide dispersion-enhanced platinum-rhodium material This is because the characteristics of may be lowered. After the hot working, it is also preferable to perform heat treatment to prevent the occurrence of cracking during cold working, and to perform cold working to obtain a recrystallized heat treatment structure through thickness control and final heat treatment.
  • the rolling reduction rate during rolling is preferably 40 to 90%. If the reduction ratio is less than 40%, the processing force is low, so recrystallization may not occur even after heat treatment. If the reduction ratio is higher than 90%, the material may be damaged due to high processing force.
  • the recrystallization heat treatment condition is less than 1 ° C temperature and less than 1 hour, recrystallization of microstructures can be suppressed, and when the temperature exceeds 1400 ° C and 5 hours, grains and oxides are coarsened to deteriorate high temperature strength. There is concern.
  • the relative density of the final product prepared through the above-described post-processing step is 99% or more.
  • the present invention provides a platinum-rhodium alloy material for oxide dispersion strengthening for producing LCD Glass prepared by the method described above.
  • the platinum-rhodium alloy material for strengthening the oxide dispersion has a relative density comparable to that of the platinum-rhodium alloy material manufactured by conventional hot press, and it can be seen that the stretched grains are maintained even after the heat treatment (FIG. 3 to 4).
  • the platinum-rhodium alloy material according to the present invention compared with the alloying material of the comparative example prepared by other conventional methods, showed a similar grain size, it was confirmed that it has a better high temperature tensile strength (Figs. 6-7 and See Table 2).
  • Melt Spinning was used for the ingot manufactured by vacuum melting, and the prepared ingot was charged into the nozzle of the melt spinning equipment, and then the melt flowed by pressing Ar Gas was rotated at 2500 rpm.
  • the metal sheet was fabricated by engraving on the surface of the Cu Wheel.
  • the prepared platinum thin plate was subjected to atmospheric heat treatment for 1 hour in the range of 1000 ° C. for oxide formation and dispersion of the additive element for oxide.
  • As a result of TEM analysis of the oxide dispersion-enhanced platinum-rhodium alloy thin plate manufactured by the present invention it was found that about 200 nm of Zr oxide particles which appeared to be white were dispersed (see FIG. 5).
  • 500t of Pt-10wt% R-0.3wt% Zr ingot was prepared using a vacuum high frequency induction furnace.
  • a vacuum pump attached to the plasma equipment was used to reduce the pressure to ⁇ 3 torr, and then plasma was formed using Ar as a reaction gas.
  • the ingot was melted, and the plasma power was further increased.
  • the prepared powder was placed in a square molded carbon mold and heat-treated at 1300 ° C. for 2 hours in an argon (Ar) atmosphere to prepare a molded article, and at 1400 ° C. and 2 in air to form oxides of oxide elements of the prepared molded article. Heat treatment was carried out for a time.
  • the oxidation-treated specimen is 1300 ° at C for 2 hours was conducted to hot pressing to 20 MPa pressure, the second 1300 ° C in a type reinforced end-oxide distributed through a hot rolling, cold rolling and heat treatment for the high density secured in order to secure a high density
  • a platinum rhodium material was prepared.
  • the platinum-rhodium alloy prepared in the comparative example shows 170 MPa (see Figure 7a)
  • the platinum-rhodium alloy of the present invention prepared in Example has a high silver tensile strength of 212 MPa is shown (see FIG. 7B). Therefore, it was confirmed that the tensile strength of the platinum-rhodium alloy of the present invention produced by the discharge plasma sintering method (SPS) was superior to the conventional method.
  • SPS discharge plasma sintering method
  • the average grain sizes of the platinum-rhodium alloys prepared in Comparative Example and Example were 23.3 and 23.1 // m, respectively (see Table 2).
  • the platinum-rhodium alloy material for oxide dispersion strengthening of the present invention not only exhibits grain size comparable to that of the platinum-rhodium alloy material manufactured by hot press sintering, but also has excellent high temperature tensile strength. (See Figures 6-7).

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacture Of Alloys Or Alloy Compounds (AREA)
  • Powder Metallurgy (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

La présente invention concerne la fabrication d'un alliage platine-rhodium renforcé par dispersion d'oxyde destiné à être utilisé pour un dispositif de fabrication de verre à cristaux liquides et, plus précisément, concerne un nouveau procédé de fabrication d'un matériau d'alliage platine-rhodium renforcé par oxyde par fabrication d'une plaque mince d'alliage de platine par utilisation d'un procédé de filage à l'état fondu, réalisation d'une oxydation interne uniquement à l'aide d'un traitement thermique atmosphérique dans un temps court, fixation de la densité par utilisation d'un procédé de frittage par plasma d'étincelle (SPS) et enfin, dispersion minutieuse d'un oxyde à haute densité par un post-traitement. Comparativement à un processus classique de fabrication d'un alliage platine-rhodium par utilisation d'une presse à chaud pour fixer la densité, la présente invention peut présenter des effets de réduction du temps de traitement et des coûts.
PCT/KR2013/009983 2013-10-29 2013-11-06 Procédé de fabrication d'alliage platine-rhodium renforcé par dispersion d'oxyde pour la fabrication de verre à cristaux liquides par utilisation d'un frittage par plasma d'étincelles Ceased WO2015064808A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
KR10-2013-0129043 2013-10-29
KR1020130129043A KR101560455B1 (ko) 2013-10-29 2013-10-29 방전 플라즈마 소결을 이용한 LCD Glass 제조용 산화물 분산 강화형 백금­로듐 합금의 제조 방법

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WO2015064808A1 true WO2015064808A1 (fr) 2015-05-07

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Cited By (2)

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CN110004317A (zh) * 2019-05-08 2019-07-12 昆明贵金属研究所 一种氧化物强化铂铑基复合材料的电弧熔炼制备方法
CN110106386A (zh) * 2019-05-08 2019-08-09 昆明贵金属研究所 氧化物强化铂铑基复合丝材的制备方法及铂铑基复合丝材

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TWI803462B (zh) 2016-05-06 2023-06-01 美商康寧公司 物件形成方法

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JP2005163069A (ja) * 2003-11-28 2005-06-23 Tanaka Kikinzoku Kogyo Kk 強化白金材料の製造方法
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Publication number Priority date Publication date Assignee Title
CN110004317A (zh) * 2019-05-08 2019-07-12 昆明贵金属研究所 一种氧化物强化铂铑基复合材料的电弧熔炼制备方法
CN110106386A (zh) * 2019-05-08 2019-08-09 昆明贵金属研究所 氧化物强化铂铑基复合丝材的制备方法及铂铑基复合丝材
CN110004317B (zh) * 2019-05-08 2020-11-24 昆明贵金属研究所 一种氧化物强化铂铑基复合材料的电弧熔炼制备方法
CN110106386B (zh) * 2019-05-08 2021-02-12 昆明贵金属研究所 氧化物强化铂铑基复合丝材的制备方法及铂铑基复合丝材

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