US20130101456A1 - Method for Producing Shaped Bodies from Aluminium Alloys - Google Patents

Method for Producing Shaped Bodies from Aluminium Alloys Download PDF

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Publication number
US20130101456A1
US20130101456A1 US13/638,772 US201113638772A US2013101456A1 US 20130101456 A1 US20130101456 A1 US 20130101456A1 US 201113638772 A US201113638772 A US 201113638772A US 2013101456 A1 US2013101456 A1 US 2013101456A1
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United States
Prior art keywords
binder
debinding
carried out
thermal debinding
aluminum
Prior art date
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Abandoned
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US13/638,772
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English (en)
Inventor
Herbert Danninger
Christian Gierl
Branislav Zlatkov
Johan Ter Maat
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Technische Universitaet Wien
Rubert Fertinger GmbH
Rupert Fertinger GmbH
BASF SE
Original Assignee
Technische Universitaet Wien
Rubert Fertinger GmbH
BASF SE
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Application filed by Technische Universitaet Wien, Rubert Fertinger GmbH, BASF SE filed Critical Technische Universitaet Wien
Assigned to TECHNISCHE UNIVERSITAT WIEN, RUBERT FERTINGER GMBH, BASF SE reassignment TECHNISCHE UNIVERSITAT WIEN ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: ZLATKOV, BRANISLAV, TER MAAT, JOHAN, DANNINGER, HERBERT, GIERL, CHRISTIAN
Assigned to BASF SE, TECHNISCHE UNIVERSITAT WIEN, RUPERT FERTINGER GMBH reassignment BASF SE CORRECTIVE ASSIGNMENT TO CORRECT THE ASSIGNEE NAME AND ASSIGNEE ADDRESS PREVIOUSLY RECORDED ON REEL 029465 FRAME 0158. ASSIGNOR(S) HEREBY CONFIRMS THE ASSIGNMENT OF ASSIGNOR'S INTEREST. Assignors: ZLATKOV, BRANISLAV, TER MAAT, JOHAN, DANNINGER, HERBERT, GIERL, CHRISTIAN
Publication of US20130101456A1 publication Critical patent/US20130101456A1/en
Abandoned legal-status Critical Current

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    • 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
    • B22F3/12—Both compacting and sintering
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • 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
    • B22F3/20—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces by extruding
    • 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
    • B22F3/1017—Multiple heating or additional steps
    • B22F3/1021—Removal of binder or filler
    • 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
    • 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
    • B22F3/22—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip
    • B22F3/225—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces for producing castings from a slip by injection molding
    • 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
    • B22F3/24—After-treatment of workpieces or articles
    • 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
    • C22C1/0408—Light metal alloys
    • C22C1/0416—Aluminium-based alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent

Definitions

  • the metal injection molding technology experienced a boom in recent years and has become an established technology for producing complex small parts, generating a worldwide annual turnover of approximately EUR 1 billion.
  • the combination of the molding technology applied for plastic injection molding with various materials used in powder technology has opened up interesting new markets for many materials.
  • the production method essentially comprises the process steps described below.
  • a feedstock in the form of an injectable granulate which consists of metal powder and a plastic component comprising at least two intimately mixed polymer components, is produced.
  • This feedstock is then molded by plastic injection molding machines to obtain molded articles.
  • These so called “green bodies” usually contain approx. 40% by volume of a plastic binder, which is largely removed in the subsequent so called debinding (or “debindering”) step.
  • a residual binder component, the so called “backbone” remains and guarantees the residual strength of the article after defending.
  • the defending can be achieved in various ways, for example thermally, using solvents, catalytically, etc., the selected process being carefully adapted to the plastic binder used in the granulate.
  • the article After debinding, the article, the so called “brown body”, is subjected to a sintering process, in the first step of which the residual “backbone” binder is usually thermally removed, whereafter the article is sintered and shrinks to form a nearly compact metal component.
  • This technology is currently applied to high- and low-alloy steels, precious metals, hard metals, but also to ceramics.
  • a particular difficulty in connection with the above described processing of aluminum relates to the relatively low melting point of aluminum (660° C.), which is further lowered when alloying elements such as tin are added thereto. This results in the problem that debinding of the plastic component has to be completed at very low temperatures, making the suitable process time frame often too short for guaranteeing the plastic component's complete removal. If the plastic component is not completely removed, undesired reactions of organic residual components with metal components may take place, which interfere with the sintering process and thus impair the mechanical characteristics obtainable by the method.
  • the aim of the present invention consisted in developing a metal injection molding process for producing molded articles of aluminum materials with good mechanical characteristics in a simple and reproducible way.
  • the inventors have achieved this aim by providing a method for producing molded articles based on aluminum alloys by metal injection molding, said method comprising the following steps:
  • the method of the invention being characterized in that the binder is completely removed in step c), wherein thermal debinding is carried out to remove the (residual) binder, optionally after having carried out one or more previous debinding steps, said thermal debinding being carried out in an atmosphere containing at least 0.5% by volume of oxygen, whereafter the thus obtained, completely debound (or debinded or debindered) brown body is sintered.
  • This method yields highly pure molded articles of aluminum alloys, as, due to the complete removal of the binder in step c), there are no undesired reactions of the plastic material with the alloying metals.
  • the complete removal of the binder is achieved due to the presence of oxygen in the atmosphere, even at relatively low temperatures.
  • the inventors have found that a small portion of oxygen, of at least 0.5% by volume, does not significantly increase the oxidation of the aluminum, but contributes to a faster and complete debinding.
  • an oxygen content for example, between 20 and 100% by volume is applied, which means that it is even possible to use pure O 2 gas.
  • the aluminum alloy contains one or more other metals which are not subject to any specific limitations.
  • the alloy partners are preferably selected from the group consisting of magnesium, copper, silicon, and manganese, and are particularly preferably contained at proportions of 0.5 to 25% by weight, in order to obtain molded articles having the desired characteristics.
  • Metals such as bismuth, tin, lead, indium, or zinc, or alloys such as Wood's metal, which have significantly lower melting points and which, in some cases, may serve as sintering aids lowering the temperature at which melting starts, are not required according to the present invention, but may still be added as alloying partners, if desired, in order to obtain sintered bodies of the respective alloys. It is particularly advantageous to use the other metals in the form of alloys with aluminum, i.e. as so-called master alloy powders.
  • polyacetal-based binders e.g. poly(oxymethylene) (POM) binders
  • POM poly(oxymethylene)
  • the binder it is desirable for the binder to have a high polyacetal percentage, consisting preferably of 50 to 95%, even more preferably of 80 to 90%, of polyacetal to promote the fast and complete removability at low temperatures and in the presence of oxygen.
  • binder systems based on wax and polymers may be used, the wax as the main component being removed by a preceding solvent debinding, i.e. before carrying out the thermal debinding in the presence of oxygen according to the invention.
  • the debinding in step c) of the method of the invention may comprise a single thermal debinding step in the presence of oxygen in which the binder is completely removed.
  • one or more preceding debinding steps may be carried out to remove the main proportion of the binder, followed by the thermal debinding step of the invention to remove the residual binder in the presence of oxygen.
  • a preceding debinding step may also be a thermal debinding step—in the absence or also in the presence of oxygen. This means that it is also possible to carry out a multi-step thermal debinding process using different process parameters for debinding—for example at different temperatures or in different atmospheres, for example without and with oxygen or with air or with pure oxygen, etc.
  • catalytic debinding and/or solvent debinding is carried out before the thermal debinding to remove the residual binder in the presence of oxygen in step c).
  • the main part of the binder is already removed from the composition so that only the “backbone” component remains to be removed by the subsequent thermal debinding.
  • Catalytic debinding is preferably carried out in the presence of at least one acid selected from nitric acid, oxalic acid, formic acid, and acetic acid, as these acids accelerate the complete removal of the preferred polyacetal binders by acidolysis without leading to undesired side reactions with the alloy components.
  • the main part of the binder is removed by extraction with a suitable solvent or mixed solvent, e.g. acetone, n-heptane, water, etc.
  • a suitable solvent or mixed solvent e.g. acetone, n-heptane, water, etc.
  • the thermal debinding process for removing the residual binder in step c) is carried out at a relatively low temperature in order to avoid oxidation reactions, particularly of the aluminum contained in the powder mixture.
  • a relatively low temperature herein refers to a temperature which is significantly lower than the melting point of aluminum, preferably below 500° C., more preferably between 100 and 420° C. It is particularly preferred to set a temperature profile optimized for the respective powder mixture, providing for a heating rate of not more than 5 K/min, more preferably of not more than 1 to 2 K/min. In this way, the mixture to be debound is heated gently and homogeneously.
  • the sintering step d) of the method of the invention is not subject to any specific limitations, except for the fact that the binder has to be completely removed beforehand. It is preferred, however, to carry out the sintering step upon formation of a liquid phase, as will be described in further detail below.
  • step d) the completely debound brown body is sintered while forming a liquid phase.
  • the liquid phase which is partly intermediary, but mainly stationary, i.e. is in a state of thermodynamic equilibrium with the solid Al phase, establishes the required contact between the metals in the powder mixture via microcracks, micropores or similar “openings” in the oxide skins of the metal powder particles and by creeping under the oxide skins, and thus it promotes the formation of a highly compacted sintered body out of the completely debound brown body.
  • step d) It is particularly preferred to carry out the sintering in step d) at a temperature between the solidus and the liquidus temperatures of the respective aluminum alloy, so that, at every point in time during the sintering process, a portion of the alloying-metals, which can be controlled by selecting the adequate temperature profile, is in a liquid state, which efficiently prevents a loss of dimensional stability.
  • the composition of the respective atmospheres in the individual steps of the inventive method is not subject to any specific limitations, except for the presence of oxygen for thermal debinding in step c); those skilled in the art are capable of selecting the atmosphere which is best suited for the respective powder mixture for each step, vacuum also being an option.
  • the sintering step d) is preferably carried out in an extremely dry, nitrogen-containing atmosphere, i.e. in pure nitrogen, under normal pressure or under reduced pressure (“partial pressure sintering”), or in a mixture of nitrogen and pure inert gas (helium, argon), preferably having a dew point below ⁇ 40° C., as the presence of nitrogen significantly promotes the powder particles' wettability with the developing metal melt.
  • the sintering step may be optionally followed by a suitable additional treatment by which the finished molded parts are kept in the desired shape. It is, for example, possible to apply the known hot isostatic pressing (HIP) process in order to achieve the desired final density of the molded parts. In this process, residual pores which are still present after the sintering step are sealed under the influence of external gas pressure and high temperatures.
  • HIP hot isostatic pressing
  • FIG. 1 is a photograph of the green body (top) and of the sintered body (bottom) obtained therefrom in Example 9.
  • FIG. 2 is a photograph of the green body (left) and the sintered body (right) obtained therefrom in Example 10.
  • the feedstock was at first filled into the funnel of the injection molding machine.
  • the injection molding process for producing the green bodies comprised the following steps: Using a heated injection cylinder with a rotating screw inside, the pretreated charging material was plastified and predosed according to preset parameters (including, for example, rotational speed, dosing volume, back pressure, etc.). Then the predosed amount was injected into an adequately tempered instrument. Depending on the feedstock and the binder used therein, the plastification temperature in the injection cylinder ranged between 120 and 220° C., while the temperature inside the instrument was between 25 and 140° C. After a sufficiently long cooling period, the injection molding instrument was opened and the green body was discharged from and taken out of the instrument using a handling device.
  • a commercially available metal powder mixture (Alumix® 231 from Ecka), consisting of aluminum with 14% by weight of silicon, 2.5% by weight of copper, and 0.6% by weight of magnesium, was thoroughly mixed with a solvent binder consisting of wax/thermoplastic to obtain a feedstock.
  • This feedstock was first debound by solvent extraction using acetone in a 60 l oven at 45° C. in 12 h.
  • the thus obtained brown body contained approximately 14.5% by weight of residual binder, which was subsequently removed by thermal debinding according to the invention in an atmosphere containing pure oxygen, applying a temperature profile ranging from 150° C. to 320° C. for 1 h and then from 320 to 420° C. for 1.5 h.
  • the thus completely debound brown body was then sintered within 1 h at 560° C. in pure nitrogen (dew point: ⁇ 50° C.).
  • the bars were sintered for 1 h in pure nitrogen, the oven temperature being set to 665° C. and amounting to approximately 630° C. inside the oven.
  • Feedstock component Percentage (% by weight) Aluminum powder 70.1 Magnesium powder 2.2 POM binder 24.0 Surfactant* 3.7 100.0 *ethoxylated C 13 -C 15 -oxoalcohol having 7 EO-units
  • Feedstock component Percentage (% by weight) Aluminum powder 70.1 Magnesium powder 2.2 POM binder 24.0 Surfactant* 3.7 100.0 *ethoxylated C 13 -C 15 -oxoalcohol having 7 EO-units
  • catalytic debinding was carried out in a 50 l oven using 2% by volume of HNO 3 in 500 l/h of nitrogen (technical grade) at 140° C. for 10 h. Weight loss: 22.1%. Thereafter, bead-like outgrowths were observed on the surface, which were assumed to have been formed by the reaction of Mg with HNO 3 .
  • thermal debinding was carried out at a temperature of up to 420° C. in pure nitrogen within 1 hour, as described in Example 3, again followed by sintering for 1 h at an oven temperature set to 665° C.
  • Feedstock component Percentage (% by weight) Aluminum powder 70.1 Magnesium powder 2.2 POM binder 24.0 Surfactant* 3.7 100.0 *ethoxylated C 13 -C 15 -oxoalcohol having 7 EO-units
  • catalytic defending according to Example 4 was carried out at 140° C. for 24 h, using 80 g anhydrous oxalic acid on a sublimation dish instead of HNO 3 . Weight loss: 23.0% .
  • oxalic acid there were no outgrowths appearing on the surface.
  • thermal debinding and sintering were also carried out according to Example 4.
  • catalytic debinding was carried out according to Example 5. Weight loss: 25.2%. Thereafter, thermal debinding and sintering were carried out according to Example 4, applying an oven temperature set to 560° C.
  • Feedstock component Percentage (% by weight) Aluminum powder 68.0 Master alloy powder* 4.3 POM binder 24.0 Surfactant** 3.7 100.0 *master alloy consisting of 50/50 aluminum and magnesium **ethoxylated C 13 -C 15 -oxoalcohol having 7 EO-units
  • Feedstock component Percentage (% by weight) Aluminum powder 68.0 Master alloy powder* 4.3 POM binder 24.0 Surfactant** 3.7 100.0 *master alloy consisting of 50/50 aluminum and magnesium **ethoxylated C 13 -C 15 -oxoalcohol having 7 EO-units
  • thermal debinding was carried out according to Example 5. Weight loss: 23.7%. Thereafter, thermal debinding and sintering were carried out according to Example 4.
  • Feedstock component Percentage (% by weight) Aluminum powder 67.1 Master alloy powder* 4.3 POM binder* 25.8
  • Feedstock component Percentage (% by weight) Aluminum powder 67.1 Master alloy powder* 4.3 POM binder 25.8
  • the method of the invention is thus capable of providing sintered bodies of aluminum alloys by injection molding, which are suitable for practical applications in different fields, including the fields of transport, construction, mechanical engineering, packaging industry, iron and steel industries, electronic engineering, household appliances, etc., for example for dissipating heat as heat sinks in electronic devices, or as components of air conditioning systems.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Powder Metallurgy (AREA)
US13/638,772 2010-04-01 2011-03-31 Method for Producing Shaped Bodies from Aluminium Alloys Abandoned US20130101456A1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
ATA534/2010 2010-04-01
ATA534/2010A AT509613B1 (de) 2010-04-01 2010-04-01 Verfahren zur herstellung von formköpern aus aluminiumlegierungen
PCT/AT2011/000157 WO2011120066A1 (de) 2010-04-01 2011-03-31 Verfahren zur herstellung von formkörpern aus aluminiumlegierungen

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US (1) US20130101456A1 (enrdf_load_stackoverflow)
EP (1) EP2552630B1 (enrdf_load_stackoverflow)
JP (1) JP5956419B2 (enrdf_load_stackoverflow)
KR (1) KR20130079373A (enrdf_load_stackoverflow)
AT (1) AT509613B1 (enrdf_load_stackoverflow)
DK (1) DK2552630T3 (enrdf_load_stackoverflow)
ES (1) ES2639134T3 (enrdf_load_stackoverflow)
HU (1) HUE035814T2 (enrdf_load_stackoverflow)
PL (1) PL2552630T3 (enrdf_load_stackoverflow)
SG (1) SG184423A1 (enrdf_load_stackoverflow)
WO (1) WO2011120066A1 (enrdf_load_stackoverflow)

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CN103769587A (zh) * 2013-11-28 2014-05-07 王利民 一种金属3d打印法产品生产方法及设备
US20160102388A1 (en) * 2013-05-07 2016-04-14 Charles Grant Purnell Aluminium alloy products, and methods of making such alloy products
US9556072B2 (en) 2009-06-25 2017-01-31 Basf Se Process for the continuous thermal removal of binder from a metallic and/or ceramic shaped body produced by injection molding, extrusion or pressing using a thermoplastic molding composition
CN112014538A (zh) * 2019-05-29 2020-12-01 波音公司 测试金属注塑成型部件的材料性质的单块前体测试试样
US11097456B2 (en) * 2018-06-21 2021-08-24 Shenzhen Future Technology Co., Ltd Preparation method for hollow radiator and hollow radiator
CN114131021A (zh) * 2021-12-01 2022-03-04 湖南英捷高科技有限责任公司 一种Al-Si-Mg系铝合金的金属注射成形方法
WO2023156610A1 (en) 2022-02-18 2023-08-24 Basf Se A process for the treatment of at least one three-dimensional green body
CN118832158A (zh) * 2024-09-24 2024-10-25 成都增谊科技有限公司 一种3d打印回收不锈钢粉末的热解酸洗复合方法
US12233469B2 (en) 2019-05-29 2025-02-25 The Boeing Company Monolithic precursor test coupons for testing material properties of metal-injection-molded components and methods and apparatuses for making such coupons

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CN104057090A (zh) * 2013-03-20 2014-09-24 江苏天一超细金属粉末有限公司 打印金属、陶瓷制品的金属、陶瓷粉末与聚合物混融材料及聚合物在成型品中的脱除方法
CN104227002A (zh) * 2013-06-19 2014-12-24 东莞市事通达机电科技有限公司 一种铝粉冶金注射成型工艺
TWI669330B (zh) * 2018-05-23 2019-08-21 晟銘電子科技股份有限公司 金屬射出成型射料組合物、成型體及其製備方法
US11229951B2 (en) 2019-05-29 2022-01-25 The Boeing Company Monolithic precursor test coupons for testing material properties of metal-injection-molded components and methods and apparatuses for making such coupons
CN113878116A (zh) * 2021-10-11 2022-01-04 深圳艾利佳材料科技有限公司 一种基于仿形治具的薄壁长条零部件的烧结方法

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