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WO2003037552A1 - Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane - Google Patents

Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane Download PDF

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Publication number
WO2003037552A1
WO2003037552A1 PCT/SG2001/000226 SG0100226W WO03037552A1 WO 2003037552 A1 WO2003037552 A1 WO 2003037552A1 SG 0100226 W SG0100226 W SG 0100226W WO 03037552 A1 WO03037552 A1 WO 03037552A1
Authority
WO
WIPO (PCT)
Prior art keywords
elemental
alloy
time period
temperature
metal powders
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/SG2001/000226
Other languages
English (en)
Inventor
Qingfa Li
Banghong Hu
Chee Mun Choy
Suxia Zhang
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.)
Agency for Science Technology and Research Singapore
Singapore Institute of Manufacturing Technology
Original Assignee
Agency for Science Technology and Research Singapore
Singapore Institute of Manufacturing Technology
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 Agency for Science Technology and Research Singapore, Singapore Institute of Manufacturing Technology filed Critical Agency for Science Technology and Research Singapore
Priority to US10/493,803 priority Critical patent/US20050163646A1/en
Priority to PCT/SG2001/000226 priority patent/WO2003037552A1/fr
Publication of WO2003037552A1 publication Critical patent/WO2003037552A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

Links

Classifications

    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C14/00—Alloys based on titanium
    • 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
    • B22F3/14—Both compacting and sintering simultaneously
    • 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
    • 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
    • C22C1/045—Alloys based on refractory metals
    • C22C1/0458—Alloys based on titanium, zirconium or hafnium
    • 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
    • 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 relates to methods for the production of articles, particularly shaped articles, from alloys which contain Sn and/or Ti.
  • the invention provides, in various aspects, methods which include semi-solid metal powder forming, solid state metal powder diffusion and metal powder preform forming followed by hot pressing.
  • Titanium is the fourth most abundant structural metal in the crust of the earth after aluminum, iron and magnesium. Due to their superior strength to weight ratios, excellent corrosion and erosion resistance and high heat transfer efficiency, titanium and its alloys have proven to be some of the most appropriate material choices for a wide variety of critical applications in the aerospace, marine and automotive industries. With improvements in titanium and titanium alloy production, the cost for titanium and its alloys in some regions of the world has been dramatically reduced. The cost of Ti powders is equivalent to the cost of the stainless steel powders which are commonly used in the powder metallurgy (PM) and powder injection molding (PIM) industries world wide. As such, the use of titanium and its alloys has rapidly expanded to include applications in the pharmaceutical and chemical areas as well as in nuclear power plants, food, and medical prostheses. Commercial applications are also seen in sporting equipment, fashion and apparel, such as golf clubs, bicycle frames, watch cases, jewellery, eyeglasses and pens.
  • PM powder metallurgy
  • PIM powder injection molding
  • titanium particularly in the liquid state, has a very high chemical activity. It reacts strongly with oxygen, nitrogen, hydrogen, water and carbon monoxide/dioxide and also reacts with almost all the refectory crucible materials at high temperatures. Therefore, melting and casting must be carried out in special crucibles under a very high vacuum. After casting, expensive post-machining is often required to achieve the desired final dimensions. In addition, for high performance applications, hot isotropic pressing (HIP) of the castings is normally required in order to completely eliminate casting porosity. All of these barriers result in a very high fabrication cost, which limits the widespread application of titanium alloys to a great extent.
  • HIP hot isotropic pressing
  • Powder metallurgy has been evaluated as another means of producing articles of titanium alloys.
  • this process generally involves complicated HIP compaction methods which makes it difficult for general applications.
  • SSMF Semi-solid metal forming
  • SSMF Semi-solid metal forming
  • the process relies on the thixotropic behavior of the semi-solid slurries containing non-dendritic solid particles which are able to flow like viscous liquids when a shear force is applied.
  • This peculiar flow behavior has led to the development of some novel forming processes, such as so called thixo-casting and thixo-molding, for fabrication of near-net shaped components with high performance.
  • Mass production is being carried out in the United States of America and Europe with a growing trend. Due to the process characteristics, the current applications are only limited to certain Al and Mg alloys.
  • the invention advantageously provides a semi-solid metal powder forming technology for fabricating net-shaped and miniature titanium alloy components with low cost and high dimensional accuracy. As such, industry may advantageously benefit in being able to produce titanium alloy components cost effectively with enhanced productivity.
  • a method of forming an article from a tin-containing alloy comprising the steps of:
  • the elemental metal powders may include at least Ti and Sn powders, optionally with other metal powders.
  • the elemental metal powders include at least Ti, Sn and Al powders.
  • the elemental metal powders include Sn powder in an amount of at least 2 wt% based on the total weight of the elemental metal powders.
  • the elemental metal powders include Sn powder in an amount of from 2-12 wt% based on the total weight of the elemental metal powders.
  • the alloy include any alloy of Sn, but is preferably directed to alloys of Sn with Al and/or Ti.
  • the invention of this aspect may be considered to be a semi- solid metal powder forming process for Sn containing alloys given the temperature of injecting step (a) of 240°C.
  • the pressurising step (b) includes applying a pressure of from 1000 to 2800 psi for a time period of from 0.5 to 3 minutes.
  • alloying step (c) includes alloying the green part at a temperature of from 1250 to 1350°C for a time period of from 30 to 150 minutes.
  • a method of forming an article from a titanium-containing alloy comprising the steps of:
  • step (c) alloying the green part at a predetermined temperature for a predetermined time period to form the article; wherein the predetermined temperature of injecting step (a) is greater than about
  • the elemental metal powders include Sn powder, and is greater than about 350°C if the elemental metal powders include Al powder.
  • the elemental metal powders include Ti and Al powders and the predetermined temperature of injecting step (a) is between 450 and
  • the predetermined pressure in the pressurizing step (b) is from 2000 to 3000 psi and the predetermined time period in step (b) is from 120 to 480 minutes.
  • This embodiment may therefore be considered a solid state diffusion process for Ti-Al alloys.
  • the invention provides a method of forming an article from an alloy, the method comprising the steps of:
  • this aspect of the invention includes a process which involves an initial step of forming a preform followed by, generally, a semi-solid state metal powder forming process or a solid state metal powder diffusion process.
  • pressurizing step (b) and alloying step (c) may include either of the processes described for the first and second aspects of the invention.
  • Figure 1 illustrates graphically a Ti-Al binary phase diagram.
  • Figure 2 illustrates graphically a Ti-Sn binary phase diagram.
  • Figure 3 illustrates a Ti-6Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1350 °C v lhr.
  • Figure 4 illustrates a Ti-6Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1400 °C v lhr.
  • Figure 5 illustrates Ti-6Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1450 °C v lhr.
  • Figure 6 illustrates Ti-9Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1350 °C v lhr.
  • Figure 7 illustrates Ti-9Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1400 °C 2.5hr (spherical Ti powders).
  • Figure 8 illustrates a Ti-12Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1400 °C v lhr.
  • Figure 9 illustrates Tii-5Al-2.5Sn elemental blended alloy formed by semi-solid forming followed by alloying treatment at 1350 °C v lhr.
  • Figure 10 illustrates Ti-8A1 fabricated by semi-solid state diffusion followed by alloying treatment 1350 °C for 1 hr. (predominated alpha-Ti structure).
  • Figure 11 XRD analysis results for Ti-9Sn elemental blended alloy formed by semi-solid metal powder forming process prior to alloying.
  • Figure 12 XRD analysis results for Ti-9Sn elemental blended alloy formed by semi-solid metal powder forming process followed by alloying at a temperature of 1350 °C.
  • the elemental metal powders used in each of the aspects of the invention are Ti, Al and Sn. Many other elemental metal powders may be added, but for simplicity and clarification, only the above elemental metal powders have been the subject of experimental analysis. Metal Alloys and Their Blending
  • the first aspect of the invention provides advantages using semi-solid metal forming techniques with the incorporation of elemental Sn powder.
  • any alloys containing more than 2% elemental Sn powder can be formed in this method.
  • Other identified commercial and semi-commercial grades of Ti alloys, which can be processed in this way are given below by way of example only:
  • Two die sets have been designed: one a Ti-watch case which is used to verify the formability of the materials using the newly developed metal powder semi-solid forming technology of the first aspect of the invention, and the other a tensile bar which is used to verify the mechanical properties.
  • the die set used for the tensile bars was very similar to a conventional PM die set design, but was combined with heating facilities generally adopted in conventional PIM, plastic injection molding or die casting die set designs.
  • This die set used for the watchcase components was similar to a conventional PM die set design, but a full profile ejector was applied.
  • an upper part for accommodating the extra powders was designed so as to be movable such that the parts formed could be easily ejected without damage.
  • Semi-solid metal powder forming according to the first aspect of the invention was carried out using a hot plate press and a hydraulic press specifically designed and installed for this project.
  • the die set on the hot plate press could be heated to a maximum temperature of 600 °C.
  • a maximum pressure of 3000psi could be applied to the die set and held at a predetermined temperature for up to at least 10 hours.
  • All of the Ti watchcase samples were produced with this press using the designed watchcase die set. Initially, tensile bars were also produced using this small hot plate press. When the fusibilities were shown on this machine, a tensile bar die set for large press and semi-auto operation was then designed.
  • a hydraulic press was used to produce the required tensile bars for tensile property verification after initial testing on the small hot plate press.
  • the die set was heated up to 280°C and held for about 1- 5 minutes.
  • Most of the tensile bars were produced using this machine as it is very fast and easy to operate (semi-auto) whereas the small press was manual and very slow.
  • the present invention considers a number of different forming methods. These, which include powder metallurgy, solid state metal powder diffusion, semi-solid metal powder forming and metal powder forming followed by hot pressing, will be dealt with in turn below.
  • die set temperatures of greater than 100°C at applied pressure of from 2500 to 3000 psi for periods of from 1 to 8 hours have successfully produced both tensile bar and watchcase samples.
  • tensile bars For tensile bars, a group of Ti alloys containing 2 to 12 % elemental Sn metal powder was processed using a semi-solid metal powder forming process. The Sn-containing Ti alloys were put into the die set cavity which was preheated to 250 to 300°C and held under a pressure of 1000 to 2500psi for about 1 to 3 minutes. Tensile bars were successfully produced in this way.
  • the group of Sn-containing Ti alloys were put into the watchcase die cavity which was preheated temperature of 250 to 300°C and held under a pressure of 2500 to 2800psi for about 1 to 3 minutes. Watchcase samples were successfully produced in this way.
  • the metal powder alloys were firstly formed into a simple shape, similar to the final geometry of the components to be made, by conventional PM process.
  • the preforms were then processed using either a semi-solid forming or solid state diffusion process. This process is advantageously tidy and surface finish can be further improved.
  • the preforms were then processed using either a semi-solid forming or solid state diffusion process.
  • a simple shape can be formed first and then followed by progressive forming (several die set together) using either semi-solid or solid state diffusion process.
  • the above-formed tensile bars and watchcases were sintered at a temperature of from 1200 to 1450°C under vacuum and Argon.
  • the holding time was about 1 to 3 hours.
  • the sintering profiles are shown in Table 2.
  • the green part density is very close to the sintered density, the sintered density being about 98% of the theoretical density, assuming the mixed powder density is the theoretical density. It is also noted that for some alloys containing Al elemental powder, the sintered density is lower than the green part density. This may be due to the relaxation of the Al powder during sintering. It is also confirmed that for Ti- 20%A1, the sintered density is much lower than the green part density and the size of the sintered components are much larger than those of the green parts.
  • the shrinkage factor is in the range of 0.4 to 2.1 % for Ti-Sn alloys and 0.25 to 0.7% for Ti-AI-Sn alloys.
  • the binary phase diagram for Ti-Sn is given in Figure 2. As can be seen in the diagram, the final phase will be alpha-Ti, where the original composition contains less than 20 wt.% Sn, under equilibrium conditions. Again, in practice there may be some beta and other compounds present due to the sintering conditions applied.
  • the selective microstructures for Ti-6Sn, Ti-9Sn and Ti-12Sn are given in Figures 3 to 5, Figures 6 to 7 and Figure 8 respectively.
  • the microstructures mainly consist of the alpha-Ti phase with some minor compounds, which are identified by the subsequent XRD analysis.
  • the basic microstructures following sintering at temperatures in the range of 1300 to 1450°C are similar. Based on the microstructure, there are still voids present at a level of 1 to 2% which may be eliminated by optimizing the process parameters.
  • the selective microstructure for Ti-5Al-2.5Sn is shown in Figure 9. It can be seen that the microstructures are uniform and predominated by V-Ti and minor compounds identified by the subsequent XRD analysis.
  • the selective microstructures for Ti-8A1 are given in Figure 10. It can be seen that the grain size is very similar to the original particle size, which indicates that no abnormal grain size growth has taken place.
  • the percentage voids for this alloy formed by semi-solid state processing followed by sintering is relative large compared to the other alloys outlined above. The reason is that this process is very similar to the conventional PM process but only the processing temperature is increased from room to a temperature which is below the melting point of Al.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Powder Metallurgy (AREA)

Abstract

La présente invention concerne un procédé permettant la réalisation d'un article à partir d'un alliage tel qu'un alliage contenant de l'étain ou un alliage contenant du titane. Des poudres de métal élémentaire de constituants métalliques de l'alliage sont injectées dans une matrice préchauffée et une pression est appliquée pour former une pièce verte. La pièce verte est alors mise sous forme d'alliage à une température prédéterminée pendant un temps prédéterminé pour former l'article. L'invention a également pour objet un article formé grâce audit procédé.
PCT/SG2001/000226 2001-10-31 2001-10-31 Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane Ceased WO2003037552A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US10/493,803 US20050163646A1 (en) 2001-10-31 2001-10-31 Method of forming articles from alloys of tin and/or titanium
PCT/SG2001/000226 WO2003037552A1 (fr) 2001-10-31 2001-10-31 Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/SG2001/000226 WO2003037552A1 (fr) 2001-10-31 2001-10-31 Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane

Publications (1)

Publication Number Publication Date
WO2003037552A1 true WO2003037552A1 (fr) 2003-05-08

Family

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Family Applications (1)

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PCT/SG2001/000226 Ceased WO2003037552A1 (fr) 2001-10-31 2001-10-31 Procedes de realisation d'articles a partir d'alliage d'etain et/ou de titane

Country Status (2)

Country Link
US (1) US20050163646A1 (fr)
WO (1) WO2003037552A1 (fr)

Families Citing this family (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TW200932921A (en) * 2008-01-16 2009-08-01 Advanced Int Multitech Co Ltd Titanium-aluminum-tin alloy applied in golf club head
EP2236634B1 (fr) * 2009-04-01 2016-09-07 Bruker BioSpin AG Alliages à base de Sn dotés de composants fins pour fils supraconducteurs en Nb3Sn
US20170067137A1 (en) * 2015-09-07 2017-03-09 Seiko Epson Corporation Titanium sintered body and ornament
CN107234242B (zh) * 2016-03-29 2021-07-30 精工爱普生株式会社 钛烧结体、装饰品及耐热部件
US11850336B2 (en) 2020-05-22 2023-12-26 Molekule Group, Inc. UV sterilization apparatus, system, and method for aircraft air systems
JP2023544252A (ja) 2020-09-14 2023-10-23 モレキュール グループ インコーポレイテッド 統合された空気殺菌器および表面消毒器
US11779675B2 (en) 2020-10-19 2023-10-10 Molekule Group, Inc. Air sterilization insert for heating, ventilation, and air conditioning (HVAC) systems

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4432795A (en) * 1979-11-26 1984-02-21 Imperial Clevite Inc. Sintered powdered titanium alloy and method of producing same
DE19723119C1 (de) * 1997-06-03 1998-08-20 Obe Ohnmacht & Baumgaertner Verfahren zur Herstellung eines einstückigen Bauteils
US5930583A (en) * 1996-08-27 1999-07-27 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Method for forming titanium alloys by powder metallurgy

Family Cites Families (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5816090A (en) * 1995-12-11 1998-10-06 Ametek Specialty Metal Products Division Method for pneumatic isostatic processing of a workpiece
US6262150B1 (en) * 2000-06-20 2001-07-17 Honeywell International Inc. Aqueous injection molding binder composition and molding process
WO2002087808A2 (fr) * 2001-04-26 2002-11-07 International Non-Toxic Composites Corp. Materiau composite contenant du tungstene, de l'etain et un additif organique

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4432795A (en) * 1979-11-26 1984-02-21 Imperial Clevite Inc. Sintered powdered titanium alloy and method of producing same
US5930583A (en) * 1996-08-27 1999-07-27 Japan As Represented By Director General Of Agency Of Industrial Science And Technology Method for forming titanium alloys by powder metallurgy
DE19723119C1 (de) * 1997-06-03 1998-08-20 Obe Ohnmacht & Baumgaertner Verfahren zur Herstellung eines einstückigen Bauteils

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