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WO2014198380A1 - Procédé de coulée d'un objet en verre métallique - Google Patents

Procédé de coulée d'un objet en verre métallique Download PDF

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Publication number
WO2014198380A1
WO2014198380A1 PCT/EP2014/001418 EP2014001418W WO2014198380A1 WO 2014198380 A1 WO2014198380 A1 WO 2014198380A1 EP 2014001418 W EP2014001418 W EP 2014001418W WO 2014198380 A1 WO2014198380 A1 WO 2014198380A1
Authority
WO
WIPO (PCT)
Prior art keywords
alloy
metal
casting
metallic glass
model
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.)
Ceased
Application number
PCT/EP2014/001418
Other languages
German (de)
English (en)
Inventor
Miriam EISENBART
Ulrich Ernst KLOTZ
Alexander Pfund
Andreas Zielonka
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.)
VEREIN fur DAS FORSCHUNGSINSTITUT fur EDELMETALLE und METALLCHEMIE E V
Original Assignee
VEREIN fur DAS FORSCHUNGSINSTITUT fur EDELMETALLE und METALLCHEMIE E V
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by VEREIN fur DAS FORSCHUNGSINSTITUT fur EDELMETALLE und METALLCHEMIE E V filed Critical VEREIN fur DAS FORSCHUNGSINSTITUT fur EDELMETALLE und METALLCHEMIE E V
Publication of WO2014198380A1 publication Critical patent/WO2014198380A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C7/00—Patterns; Manufacture thereof so far as not provided for in other classes
    • B22C7/02—Lost patterns
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22C—FOUNDRY MOULDING
    • B22C9/00—Moulds or cores; Moulding processes
    • B22C9/12—Treating moulds or cores, e.g. drying, hardening
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D25/00—Special casting characterised by the nature of the product
    • B22D25/02—Special casting characterised by the nature of the product by its peculiarity of shape; of works of art
    • B22D25/026—Casting jewelry articles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D29/00—Removing castings from moulds, not restricted to casting processes covered by a single main group; Removing cores; Handling ingots
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/01—Layered products comprising a layer of metal all layers being exclusively metallic
    • B32B15/018—Layered products comprising a layer of metal all layers being exclusively metallic one layer being formed of a noble metal or a noble metal alloy
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C45/00—Amorphous alloys
    • C22C45/003—Amorphous alloys with one or more of the noble metals as major constituent
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/02—Tubes; Rings; Hollow bodies
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D1/00—Electroforming
    • C25D1/10—Moulds; Masks; Masterforms
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
    • B22D13/00—Centrifugal casting; Casting by using centrifugal force
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00—Electroplating: Baths therefor
    • C25D3/02—Electroplating: Baths therefor from solutions
    • C25D3/38—Electroplating: Baths therefor from solutions of copper

Definitions

  • the present invention relates to a method for casting an article of solid metallic glass (amorphous metal).
  • the present invention relates to a method for casting an article from metallic glass, with the complex and filigree items made of metallic glasses can be made comparatively inexpensive, easy and fast.
  • metal alloys after solidification from a liquid phase, exist as a crystalline phase with a regular atomic arrangement. However, some alloys can retain their irregular atomic arrangement, as in the liquid phase, in the solid phase, if the rate of cooling used to solidify is high enough to substantially or even completely increase nucleation and growth of the crystalline phase suppress. Such alloys are generally referred to as amorphous alloys or metallic glasses.
  • amorphous phases Since the first report of amorphous phases in an Au-Si system in 1960, many types of amorphous alloys have been found and put to practical use. However, most of these amorphous alloys require very high cooling rates to prevent the formation of a crystalline phase in the course of cooling from the liquid phase, since the nucleation and growth of the crystalline phase in the supercooled liquid phase proceeds rapidly. Accordingly, most of the amorphous alloys could only be in the form of a thin ribbon having a thickness of about 80 ⁇ or less, a fine wire having a diameter of about 150 ⁇ or less or a fine powder having particles having a diameter of a few 100 ⁇ or be made less.
  • metal alloys there have been found, for example, Zr and Ti-containing alloys as disclosed in US Pat. Nos. 5,288,344 and 5,735,975. Due to the comparatively low cooling rates which are required in these alloys for forming a metallic glass, ie, generally less than 10 3 K / s, by conventional casting techniques and comparatively massive objects can be obtained from metallic glasses, the thicknesses or wall thicknesses of eg have more than 500 ⁇ .
  • Such conventional casting techniques are, for example, casting in solid metal molds (permanent metal molds, molds) or investment casting (casting out method).
  • the presence of the comparatively large metal mass of the metal mold usually already ensures a sufficient cooling rate in order to solidify the metal alloy in the amorphous state.
  • the ratio between the copper mass and the mass of the melt is so great that the temperature of the copper mold only increases by a few ° C. as a result of the casting process.
  • the disadvantage of casting into solid metal molds is that their production, which is usually done by a machining on modern multi-axis high-performance milling machines, is relatively complex and therefore expensive and thus worthwhile only for large numbers.
  • a core having a low melting point (usually below 90 ° C) is coated with a molding material, the core is melted after solidification of the molding material, a metal alloy is then poured into the obtained hollow molding material, and after solidification of the Metal alloy, the mold material is removed.
  • the required cores can, for example, in a very simple manner by means of rapid prototyping (SD printer with, for example, wax or low-melting plastics than Printing material) are created so that even complicated shapes can be produced quickly and inexpensively with a relatively low cost of equipment and desired changes in the structure of the core can also be quickly realized.
  • the object of the present invention is therefore to provide a method which overcomes the above-mentioned disadvantages of the prior art and which allows cost-effective, simple and rapid casting of a comparatively solid object made of metallic glass.
  • Iron, nickel, iron-nickel alloy or nickel-cobalt alloy, on the electrically conductive coating Iron, nickel, iron-nickel alloy or nickel-cobalt alloy, on the electrically conductive coating
  • Fig. 1 shows a schematic representation of steps of the method according to the invention.
  • FIG. 2 shows a copper mold produced according to the method according to the invention in accordance with Example 1 (CT image of the filled copper mold before removal of the copper).
  • Fig. 3 shows a polished solid ring of metallic glass, which has been prepared according to Example 1.
  • Fig. 4 shows a ring of metallic glass with a complex lattice shape, which has been prepared according to Example 2.
  • the model of the object can basically consist of any materials which have a comparatively low melting point of for example 40 ° C to 90 ° C, preferably 40 ° C to 70 ° C, in particular 40 ° C to 60 ° C.
  • examples of such materials are waxes and low-melting plastics, which have melting points of eg 40 ° C to 70 ° C, so that they can be melted out of the mold at low temperatures.
  • waxes from the dental / jewelery sector such as, for example, Injection Wax - Accuflakes, Turq L Blue
  • the model is made of wax.
  • model of the article may be made by any method known to those skilled in the art, e.g. by manually processing a corresponding blank, by wax spraying in rubber or silicone molds, or preferably by rapid prototyping with a corresponding 3D printer, in which the model is built up on the basis of CAD data in layers.
  • the model of the article is rendered electrically conductive by applying an electrically conductive coating to the model for the subsequent electrodeposition step of a copper layer.
  • the electrically conductive coating is formed by applying an electrically conductive lacquer (conductive ink) or an electrically conductive layer.
  • conductive ink any known conductive ink can be used, such as a conductive ink based on silver, copper or graphite particles.
  • a conductive ink based on graphite powder is particularly preferred.
  • the galvanic application of a metal layer to the electrically conductive coating takes place in a conventional manner by so-called electroforming. Basically, metals with high thermal conductivity and high melting temperature can be used here, since melting on the mold must be avoided. In the context of the present invention, it has proven to use copper, iron, nickel, iron-nickel alloys or nickel-cobalt alloys.
  • the process of electroforming is the electrolytic deposition of metal from an aqueous solution of a salt of the metal.
  • the process is carried out in an electrolytic tank containing the metal salt solution, an anode and a cathode on which the metal is to be deposited.
  • the model of the article provided with the electrically conductive coating is connected as a cathode.
  • the copper layer to be deposited in the present process can be deposited at deposition rates of 25 ⁇ m / hour to 1000 ⁇ m / hour, preferably from 50 ⁇ m / hour to 500 ⁇ m / hour.
  • the thickness of the deposited copper layer is not particularly limited and depends substantially on the amount of heat to be dissipated during the casting process, ie, the melting temperature, the alloy used, and the thickness of the article to be produced.
  • the minimum required thickness of the deposited copper layer can be calculated by the following formula: In order to estimate the minimum required thickness of the copper mold, which is just sufficient to ensure amorphous solidification, the minimum mass of the metal mold, in particular copper mold, estimated become. Assuming a lossless process during casting (adiabatic conditions), the change in the heat energy of the melt is equal to the heat change of, for example, copper form:
  • a cooling curve can be calculated as a function of time.
  • the thermal conductivity and the heat transfer coefficient are often not for massive metallic glasses However, after some time it can be assumed that a Gieich.stemperatur Tend is reached.
  • the specific thermal conductivity c P is strictly a temperature-dependent variable, but for a rough estimate it is permissible to use the value for the solid metallic glass for the melting temperature c P BG, cast and for the copper mold the value at room temperature C P CU, RT
  • mcu and mmeit are respectively the mass of copper mold and inserted MMG (solid metallic glass), c p is the specific heat capacity, Tcast is the casting temperature, Tend is the mold weight temperature of mold and MMG after casting and RT is room temperature.
  • the copper layer has a thickness of 500 ⁇ to 4000 ⁇ , preferably from 1000 ⁇ to 4000 ⁇ and in particular from 2000 ⁇ to 4000 ⁇ .
  • a metal alloy for the present process in principle, any known to the expert metal alloy can be used, which can form a metallic glass after cooling of the melt, in particular in a layer thickness of for example at least 500 ⁇ , preferably at least 1000 ⁇ , more preferably at least 2000 ⁇ and in particular at least 3000 ⁇ .
  • the metal alloy is an Au alloy.
  • an alloy of Au49Ag5.5Pd2.3Cu26.9Sii6.3 can be mentioned here.
  • a Pt alloy, Pd alloy or Zr alloy is used.
  • Such alloys are known to those skilled in the art of solid metallic glasses.
  • an alloy of Zr59.3Cu28.8A o, 4Nbi, 5 (At%) (colloquially AMZ4) may be mentioned here.
  • Another metal alloy which can be used in the present invention is an alloy of (Zr, Ti) a (Ni, Cu, Fe) t (Be, Al, Si, B) c where a is in the range of 30 to 75 atom -% is, b is in the range of 5 to 60 atomic% and c is in the range of 0 to 50 atomic% (see WO 03/064076 A1).
  • an alloy composed of Fe: 74 to 78 at%, Mo: 2 to 6 at% and B: 20 at%, or Fe: 40 at%, Ni: 34 may also be used in the present invention to 38 atomic%, Mo: 2 to 6 atomic% and B: 20 atomic%, or Fe: 67 to 76 atomic%, Ni: 0 to 9 atomic%, Mo: 4 atomic%, C : 18 atomic% and B: 2 atomic%.
  • the melting process for providing the molten metal alloy is not particularly limited in principle, that is, both a single-stage and a two-stage melting process may be employed.
  • the metal components of the alloy are mixed in the required ratio and then melted, after which the melt is cast.
  • the two-stage melting process the Metal components of the alloy mixed in the required ratio and then melted, whereupon the melt is brought in a conventional manner in a semi-finished, for example in granule form. The semifinished product is then melted again and the resulting melt is poured.
  • the melting temperature of the finished near-eutectic alloy in the semifinished product eg Granalienform
  • the melting temperature of the individual components is significantly lower than the melting temperature of the individual components, so that in comparison to the single-stage melting process, a significantly lower melting temperature during casting is possible facilitates the required rapid cooling of the melt.
  • the molten metal alloy is provided by melting a metal alloy in granule form.
  • the process of casting in the process according to the invention is in principle not restricted to a specific process and all casting processes known to those skilled in the art can be used.
  • the casting is carried out in the process according to the invention as centrifugal casting, gravity casting or tilt casting.
  • the abovementioned casting methods and the associated advantages and disadvantages are known to the person skilled in the art and are therefore not explained in more detail here.
  • the copper mold After the casting has been carried out and the melt has solidified to a solid metallic glass, the copper mold must be removed.
  • the process of removing the eg copper mold is in principle not limited to a particular method.
  • the copper mold can be removed mechanically if its shape is simple (for example, it has the shape of a simple ring) and if its layer thickness is small.
  • the copper mold may also be removed by chemical dissolution, usually with nitric acid, which is preferred according to the invention, in particular to solve the mold of cast articles having a more complex shape, such as a lattice form (see Figure 4).
  • Fig. 1 shows a schematic representation of steps of the method according to the invention, which has been explained above. Fig.
  • FIG. 1a shows a wax model 1 in ring form, which is used to produce a jewelry ring.
  • 1 b) shows the wax model 1 coated with the conductive ink 2 on which a copper layer 3 has been applied by electroforming (in FIG. 1 c).
  • FIG. 1d) shows a copper mold which has been obtained by melting out the wax from the wax model coated with the copper layer 3.
  • a copper mold as shown schematically in Fig. 1d), may e.g. having the shape shown in FIG.
  • Thermocouples are then additionally attached to the copper mold in order to be able to measure the outside temperature of the mold or the temperature profile during cooling.
  • the method according to the invention is characterized in an advantageous manner by a simplified demolding, whereas the detachment from divisible molds is difficult in amorphous castings. Due to the lack of shrinkage during solidification, the castings sit particularly firmly in the mold (casting close to the final shape). In addition, casting geometries are possible with the method according to the invention, which are otherwise difficult or impossible to produce with divisible shapes.
  • the present invention will be illustrated below by way of examples, which are not intended to be limiting. Examples Example 1
  • a wax model of a simple jewelry ring was made, the wax mold was created by means of silicone negative.
  • the wax model was coated with a graphite powder (Printex XE2, from Degussa, Essen).
  • the graphite powder was applied as a conductive layer with a brush on the wax model.
  • the coated with the graphite powder model was placed in an electrolytic tank and electrolytically coated with a 2000 ⁇ to 4000 ⁇ thick copper layer (see Figure 2).
  • a beaker was used as the electrolyte vessel, the electrolyte volume was 1.8 liters, the temperature was controlled by means of a contact thermometer and kept constant on the heating plate of a magnetic stirrer. The electrolyte circulation also took place with the aid of the magnetic stirrer.
  • Oxygen-free phosphorus-deoxidized anodes (copper anodes, Cu min 99.9%, P 0.04-0.06%, Galva-Metall GmbH, Rödermark) were used as the anodes.
  • a commercial electrolyte such as the electrolyte "Thru-cup EVF-R" (Umicore Galvanotechnik, Schissebisch Gmünd) was used and deposited at 2 A / dm 2 (0.42 pm / min).
  • the copper layer was removed in a solution of sulfuric acid and sodium peroxodisulfate (etching solution "Doduprint 300" (Ami Doduco, Pforzheim) 150 g / l) and the solution was dissolved at 40.degree.
  • the obtained from the copper mold preserved solid ring of solid metallic glass was finally polished.
  • the ring shown in FIG. 3 was obtained.
  • Example 2 was carried out substantially like Example 1, except that a wax ring with a complex shape (lattice shape) was used. The wax was melted out at a temperature of about 150-200 ° C. The resulting ring was not polished. The ring of metallic glass having a complex lattice shape obtained according to Example 2 is shown in FIG. Example 2 thus shows that objects made of metallic glass with a complex shape can be produced quickly and easily with the method according to the invention.
  • the metallic glasses produced by the process of the present invention are optically indistinguishable from ordinary metals, but generally harder (lower elongation at break), more corrosion resistant, and stronger (less scratch sensitive) than these. They can therefore be used wherever these property combinations are of particular importance.
  • the metallic glasses produced by the method according to the invention are therefore typically, but not exclusively, used in the jewelry industry for the production of jewelery made of precious metal alloys, in medical technology for the production of implants and medical tools, in mechanical engineering or in the electrical engineering industry for the production of high-quality components and surfaces as well as in the luxury goods industry for the production of high quality designer items as well as for the production of sporting goods, such as parts of golf clubs used.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • Adornments (AREA)

Abstract

La présente invention concerne un procédé de coulée d'un objet en verre métallique massif, comprenant les étapes suivantes : préparation d'un modèle (1) de l'objet, dépôt d'un revêtement électriquement conducteur (2) sur le modèle, dépôt galvanique d'une couche (3) d'un métal choisi parmi le cuivre, le fer, le nickel, un alliage de fer et de nickel ou un alliage de nickel et de cobalt sur le revêtement électriquement conducteur (2), élimination du modèle (1) par fusion pour donner une forme en métal, préparation d'un alliage métallique en fusion capable de former un verre métallique après refroidissement, coulée de l'alliage métallique en fusion dans la forme en métal, solidification de l'alliage métallique coulé pour donner un verre métallique massif, et retrait de la forme en métal.
PCT/EP2014/001418 2013-06-14 2014-05-27 Procédé de coulée d'un objet en verre métallique Ceased WO2014198380A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102013009975.7 2013-06-14
DE102013009975.7A DE102013009975A1 (de) 2013-06-14 2013-06-14 Verfahren zum Gießen eines Gegenstandes aus metallischem Glas

Publications (1)

Publication Number Publication Date
WO2014198380A1 true WO2014198380A1 (fr) 2014-12-18

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PCT/EP2014/001418 Ceased WO2014198380A1 (fr) 2013-06-14 2014-05-27 Procédé de coulée d'un objet en verre métallique

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DE (1) DE102013009975A1 (fr)
WO (1) WO2014198380A1 (fr)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110479961A (zh) * 2019-09-24 2019-11-22 龙南新晶钛业有限公司 一种钛合金组合铸造的工艺
WO2022175707A1 (fr) * 2021-02-17 2022-08-25 Creativity Box S.R.L. Unipersonale Procédé pour la fabrication de bijoux, en particulier pour bijoux, argenterie et bijoux fantaisie

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DE2829837A1 (de) * 1978-07-07 1980-01-17 Osaka City Giesswerkzeug und giessform zum giessen thermoplastischer kunststoffe
DE19537264A1 (de) * 1995-10-06 1997-04-10 Fraunhofer Ges Forschung Verfahren zur Herstellung dreidimensionaler Bauteile aus insbesondere metallischen Werkstoffen, Kunststoffen oder Keramikverbundwerkstoffen
DE19956464C1 (de) * 1999-11-19 2001-06-07 Ind Tech Res Inst Verfahren zum Herstellen von Präzisionsgießformen
WO2003061356A1 (fr) * 2002-01-17 2003-07-24 Elmicron Ag Matrice d'estampage destinee a fabriquer des interconnexions a haute densite et procede de fabrication correspondant
WO2004091828A1 (fr) * 2003-04-14 2004-10-28 Liquidmetal Technologies, Inc. Coulage en continu de structures de mousse d'alliages amorphes en masse

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US5288344A (en) 1993-04-07 1994-02-22 California Institute Of Technology Berylllium bearing amorphous metallic alloys formed by low cooling rates
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DE19537264A1 (de) * 1995-10-06 1997-04-10 Fraunhofer Ges Forschung Verfahren zur Herstellung dreidimensionaler Bauteile aus insbesondere metallischen Werkstoffen, Kunststoffen oder Keramikverbundwerkstoffen
DE19956464C1 (de) * 1999-11-19 2001-06-07 Ind Tech Res Inst Verfahren zum Herstellen von Präzisionsgießformen
WO2003061356A1 (fr) * 2002-01-17 2003-07-24 Elmicron Ag Matrice d'estampage destinee a fabriquer des interconnexions a haute densite et procede de fabrication correspondant
WO2004091828A1 (fr) * 2003-04-14 2004-10-28 Liquidmetal Technologies, Inc. Coulage en continu de structures de mousse d'alliages amorphes en masse

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110479961A (zh) * 2019-09-24 2019-11-22 龙南新晶钛业有限公司 一种钛合金组合铸造的工艺
WO2022175707A1 (fr) * 2021-02-17 2022-08-25 Creativity Box S.R.L. Unipersonale Procédé pour la fabrication de bijoux, en particulier pour bijoux, argenterie et bijoux fantaisie

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