US20110044841A1 - Method for producing microscopic components - Google Patents

Method for producing microscopic components Download PDF

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Publication number
US20110044841A1
US20110044841A1 US12/446,520 US44652009A US2011044841A1 US 20110044841 A1 US20110044841 A1 US 20110044841A1 US 44652009 A US44652009 A US 44652009A US 2011044841 A1 US2011044841 A1 US 2011044841A1
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United States
Prior art keywords
particles
alloy
less
phase
nickel
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Abandoned
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US12/446,520
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English (en)
Inventor
Joachim Roesler
Debashis Mukherji
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Technische Universitaet Braunschweig
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Technische Universitaet Braunschweig
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Assigned to TECHNISCHE UNIVERSITAT BRAUNSCHWEIG CAROLO-WILHELMINA reassignment TECHNISCHE UNIVERSITAT BRAUNSCHWEIG CAROLO-WILHELMINA ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: MUKHERJI, DEBASHIS, ROESLER, JOACHIM
Publication of US20110044841A1 publication Critical patent/US20110044841A1/en
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt
    • C22C19/007—Alloys based on nickel or cobalt with a light metal (alkali metal Li, Na, K, Rb, Cs; earth alkali metal Be, Mg, Ca, Sr, Ba, Al Ga, Ge, Ti) or B, Si, Zr, Hf, Sc, Y, lanthanides, actinides, as the next major constituent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/006—Methods for forging, hammering, or pressing; Special equipment or accessories therefor using ultrasonic waves
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J5/00—Methods for forging, hammering, or pressing; Special equipment or accessories therefor
    • B21J5/06—Methods for forging, hammering, or pressing; Special equipment or accessories therefor for performing particular operations
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J7/00—Hammers; Forging machines with hammers or die jaws acting by impact
    • B21J7/02—Special design or construction
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C99/00—Subject matter not provided for in other groups of this subclass
    • B81C99/0075—Manufacture of substrate-free structures
    • B81C99/0085—Manufacture of substrate-free structures using moulds and master templates, e.g. for hot-embossing
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C19/00—Alloys based on nickel or cobalt

Definitions

  • the invention relates to a method for producing microscopically small components.
  • preforms are first produced by microcasting or powder metallurgical methods. These preforms are subsequently machined by micro-machining in order to thus give them the desired final contour.
  • the object of the invention is therefore to disclose a method with which free components not bonded to a substrate and with a size of less than 10 ⁇ m can be produced.
  • the object is attained by the invention through a method with the steps (a) production of a precipitation hardenable, alloy comprising at least two phases, in which alloy a first phase forms a matrix structure in which a second phase is embedded in the form of discrete particles of a size less than 10 ⁇ m, preferably less than 1 ⁇ m; (b) dissolution of the matrix and separation of discrete particles from the alloy and (c) mechanical deformation by forging respectively a separated particle with at least one striking tool to form the desired element.
  • the advantage of the method according to the invention is that components with a size of less than 50 ⁇ m can be produced. It is furthermore advantageous that components with reproducible dimensions can be produced, since the particles used as output blocks likewise have a size that is reproducible in a high grade manner.
  • the method manages without lithographic or powder metallurgical processes, which reduces the expenditure in terms of equipment. Furthermore, the method makes it possible to produce components from a plurality of high-strength alloys, with which lithographic or powder metallurgical methods do not provide satisfactory results.
  • the term ⁇ , ⁇ ′ refers very generally to two different phases.
  • the first phase is a ⁇ phase and the second phase is a ⁇ ′ phase in terms of physical metallurgy.
  • the discrete particles are then, for example, ⁇ ′ particles.
  • a matrix structure is understood to mean that it is interconnected such that it can be dissolved and the particles contained therein, in particular the ⁇ ′ particles contained therein, can thus be separated from the ⁇ matrix.
  • the ⁇ ′ particles are separated by row-type and column-type areas in which the ⁇ phase is present.
  • the alloy has more than 10, in particular more than 100, ⁇ ′ particles, which are separated from one another by areas in which the ⁇ phase is present.
  • the size of the ⁇ ′ particles means in particular the maximum side length of a minimal cuboid envelope. To determine the size of a ⁇ ′ particle, the cuboid around the relevant ⁇ ′ particle is therefore determined, which cuboid completely surrounds the ⁇ ′ particle and has the smallest volume among all of the cuboid envelopes of this type, and the maximum side length thereof established. This side length represents the size of the ⁇ ′ particle.
  • the forging comprises in particular a freeform forging in which the separated ⁇ ′ particle is forged with a hammer on a flat base, and a die forging in which the ⁇ ′ particle is struck by a hammer in a die or is deformed or shaped between two dies.
  • the ⁇ ′ particles are embodied essentially in a cuboid form.
  • An essentially cuboid form should be understood to mean that a strict mathematical cuboid form is not necessary. Instead, it is sufficient if, for example, the longest side of a cuboid envelope of minimal volume around the relevant ⁇ ′ particle is no more than 15% longer than the shortest side of the corresponding cuboid envelope.
  • the maximum edge length of the cuboid or the cube is preferably less than 10 ⁇ m, preferably less than 1 ⁇ m. The advantage of this is that particularly small components can be produced.
  • the dissolution of the matrix is carried out chemically and/or electrochemically. Through this the matrix is dissolved particularly quickly and effectively, without the ⁇ ′ particles being excessively affected.
  • ⁇ ′ particles bonded on the metal surface are shaken off by means of ultrasound for the separation.
  • the metal surface is thereby in particular that surface of the alloy to which the ⁇ ′ particles were connected before the chemical and/or electrochemical dissolution.
  • the shaking off is carried out particularly preferably in an aqueous solution, which is subsequently centrifuged to obtain the ⁇ ′ particles. It is hereby ensured that the ⁇ ′ particles can be obtained with a high yield. At the same time ⁇ ′ particles are prevented from reaching the air, where they could possibly be inhaled.
  • the alloy is monocrystalline, in particular in individual or all ⁇ ′ particles. This results in particularly advantageous strength properties of the components produced.
  • the alloy is a nickel-based superalloy, since in this case particularly uniformly shaped and essentially cuboid ⁇ ′ particles can be produced and components with a particularly high mechanical strength are obtained.
  • Nickel-based superalloys with 1 to 9% by weight aluminum, 0-8% by weight titanium and 0-15% by weight tantalum, in particular 0-12% by weight tantalum, for example Udimet 710 with 2.3% by weight aluminum and 3% titanium or Waspaloy with 1.3% by weight aluminum and 3% titanium are particularly favorable. Alloys of this type have furthermore proven to be particularly advantageous for the production of ⁇ ′ particles.
  • the ⁇ ′ particles have an L 1 2 crystal structure.
  • the alloy is alternatively a nickel-iron alloy and the ⁇ ′ particles comprise Ni 3 Fe. In this manner, components with a particularly high ductility are obtained, which are also easy to forge.
  • the processing surface of the striking tool is smaller than 50 ⁇ m, in particular smaller than 5 ⁇ m.
  • the size of the processing surface is given as the side length of a square of equal area.
  • a manipulator with tungsten tip is used as striking tool and a silicon cantilever arm is used as an anvil.
  • the silicon cantilever arm has a flat surface.
  • at least one recess functioning as a die is provided in the silicon cantilever arm. This recess preferably has a base area, the maximum dimension of which is less than 5 ⁇ m. In this manner particularly small components can be produced.
  • the recess can be produced with a particularly high precision and in a particularly reproducible manner by nanolithography or microlithography.
  • a tungsten tip with a plateau is used, the maximum dimension of which is less than 5 ⁇ m.
  • a tungsten tip has the advantage of being sufficiently hard so as not to be deformed itself during forging.
  • the maximum dimensions of less than 5 ⁇ m furthermore make it possible to observe the forging operation, for example, through a scanning electron microscope.
  • FIG. 1 a A scanning electron microscope image of a precipitation hardenable nickel-based superalloy comprising two phases, in which a first phase ( ⁇ phase) forms a matrix structure in which a second phase is embedded in the form of discrete particles ( ⁇ ′ phase) of a size less than 10 ⁇ m,
  • FIG. 1 b A scanning electron microscope image of the alloy according to FIG. 1 a , in which the ⁇ phase has been removed,
  • FIG. 2 A diagrammatic view of a manipulator for forging within the scope of a method according to the invention.
  • FIGS. 3 a , 3 b , 3 c , 3 d and 3 e show the progress of a production method according to the invention in the form of scanning electron microscope images.
  • FIG. 1 a shows a scanning electron microscope image of a precipitation hardenable alloy, which has two phases, namely a ⁇ ′ phase 10 and a ⁇ phase 12 .
  • the ⁇ phase 12 represents a first phase and the ⁇ ′ phase 10 represents a second phase.
  • the first phase 12 forms a matrix structure, in which the second phase 10 is embedded in the form of a plurality of discrete ⁇ ′ particles 14 a , 14 b , . . . , of a size less than 10 ⁇ m.
  • the ⁇ ′ particles 14 are arranged in a row-type and column-type manner and separated from one another by the ⁇ phase 12 .
  • the structure shown in FIG. 1 a is produced by a heat treatment of a nickel-based superalloy SX-1, namely by solution annealing and precipitation hardening.
  • This nickel-based superalloy is composed of 11.6 At. % aluminum, 2.4 At. % tantalum, 6 At. % chromium, 3.5 At. % tungsten, 1.3 At. % molybdenum and a balance of nickel and unavoidable contaminants.
  • This heat treatment is carried out such that essentially cubic deposits in the form of the ⁇ ′ particles 14 of the type Ni 3 Al with an essentially identical size of 300 nm to 500 nm are obtained:
  • the alloy is heat treated such that the variance of the size distribution based on the average value is below 25%. Details on the production can be found in the article “Nano-structured materials produced from simple metallic alloys by phase separation” in Nanotechnology 16 (2005) 2176-2187.
  • the material namely the ⁇ ′ phase 10 and the ⁇ phase 12
  • the etching parameters are thereby selected such that the matrix, namely the ⁇ phase 12 , is dissolved. Further details on the etching parameters can be found in the above-referenced article.
  • the process of etching is interrupted at intervals of half an hour to two hours. The situation shown in FIG. 1 b thus results, in which the matrix in the form of they phase 12 is dissolved and the ⁇ ′ particles 14 a , 14 b , . . . remain.
  • an individual ⁇ ′ particle 14 is picked up with the aid of one or more, in the present case two, manipulators 16 , 18 (cf. FIG. 2 ) and placed by the manipulator or manipulators 16 , 18 on a silicon cantilever arm 20 .
  • the two manipulators 16 , 18 respectively have a tungsten needle 22 or 24 , which respectively end in a point 26 or 28 with a tip radius of 20 nm.
  • the manipulators 16 , 18 and the other components can be ordered from Kleindiek Nanotechnik GmbH, Reutlingen, Germany.
  • the manipulators 16 , 18 are controlled by means of a joystick and have drives 30 or 32 , by means of which the tungsten needles 22 , 24 can be positioned with a positional accuracy of 0.5 nm.
  • the ⁇ ′ particle 14 is processed by means of a striking tool 33 .
  • the striking tool 33 comprises a hammer in the form of a tungsten tip 34 .
  • the tungsten tip 34 is attached to a piezoelectric hammer drive 36 and has a positional accuracy in the direction towards the silicon cantilever arm 20 of 1 nm.
  • the hammer drive 36 , the silicon cantilever arm 20 and the two manipulators 16 , 18 are arranged in pairs with respect to one another such that the connecting line between manipulator 16 and silicon cantilever arm 20 on the one hand and manipulator 18 and tungsten tip 34 on the other hand run perpendicular with respect to one another.
  • Forces up to 2 mN can be applied with the aid of the hammer drive 36 .
  • the strength of the force applied is recorded by a force transducer 38 , which is arranged in a drive 40 for the silicon cantilever arm 20 .
  • the forging operation takes place at room temperature (23° C.).
  • the silicon cantilever arm 20 comprises an electric heating device (not shown). If desired, the ⁇ ′ particle 14 is thus brought to an increased temperature and subsequently processed. It is furthermore possible after a forging at room temperature to heat the ⁇ ′ particle 14 by means of the electric heating device in order to trigger recrystallization processes and/or to heal dislocations.
  • All of the components shown in FIG. 2 are arranged in a vacuum chamber of a scanning electron microscope (not shown).
  • the freeform forging of the ⁇ ′ particle 14 is constantly monitored with the aid of the scanning electron microscope.
  • the silicon cantilever arm 20 has a recess produced by nanolithography or microlithography.
  • This recess has a base surface, the maximum dimension of which is, for example, less than 1 ⁇ m by 1 ⁇ m.
  • a single ⁇ ′ particle 14 is separated with the aid of the manipulators 16 , 18 and placed at a position above the recess.
  • the ⁇ ′ particle 14 is struck or pressed into the die with the tungsten tip 34 as a hammer. In this manner, a deformed component with a precisely contoured surface and with a size of less than 1 ⁇ m is obtained.
  • a method of this type can be used, for example, to produce gear wheels with a size of less than 10 ⁇ m.
  • the ⁇ ′ particle 14 is placed above the die and struck partially into the die. A residue of the ⁇ ′ particle 14 remaining outside the die is subsequently removed.
  • a weaker vacuum is used, for example a moderate vacuum. It is then advantageous to set the lowest possible air humidity, for example, of less than 10%.
  • a method according to the invention can comprise the steps of a wetting of the silicon cantilever arm 20 and/or of the tungsten tip 34 with a lubricant layer.
  • This process step is advantageous if there is a risk that the component produced from the ⁇ ′ particle 14 will adhere firmly to the silicon cantilever arm 20 or to the tungsten tip after the forging.
  • the wetting with a lubricant layer is achieved, for example, in that a diffusion pump oil such as diffusion pump oil 705 from Dow Corning is evaporated so that it condenses on the silicon cantilever arm 20 or the tungsten tip 34 .
  • FIG. 3 a shows the tip 26 of the tungsten needle 22 of the manipulator 16 (cf. FIG. 2 ) in a scanning electron microscope image, by means of which the ⁇ ′ particle 14 is separated.
  • FIG. 3 b shows the tungsten tip 34 , at the tip of which the ⁇ ′ particle 14 is located.
  • the ⁇ ′ particle 14 is placed on the silicon cantilever arm 20 ( FIGS. 3 c and 3 d ) and subsequently deformed on the silicon cantilever arm 20 with the tungsten tip 34 ( FIG. 3 e ) so that a component is obtained.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Forging (AREA)
  • Sampling And Sample Adjustment (AREA)
  • Powder Metallurgy (AREA)
  • Compounds Of Unknown Constitution (AREA)
  • Manipulator (AREA)
US12/446,520 2006-10-28 2006-10-28 Method for producing microscopic components Abandoned US20110044841A1 (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
PCT/DE2006/001915 WO2008052494A1 (de) 2006-10-28 2006-10-28 Verfahren zur herstellung mikroskopisch kleiner bauelemente

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US20110044841A1 true US20110044841A1 (en) 2011-02-24

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US (1) US20110044841A1 (de)
EP (1) EP2086701B1 (de)
AT (1) ATE537920T1 (de)
DE (1) DE112006004191A5 (de)
WO (1) WO2008052494A1 (de)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10525207B2 (en) 2010-07-22 2020-01-07 Becton, Dickinson And Company Dual chamber syringe with retractable needle

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5994820A (en) * 1994-11-15 1999-11-30 Kleindiek; Stephan Electromechanical positioning unit
US20060138897A1 (en) * 2003-07-04 2006-06-29 Peter Hess Tool head comprising piezoelectric actuators

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100543179B1 (ko) * 2004-04-10 2006-01-20 한국기계연구원 3차원 형상의 마이크로 부품 제작방법

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5994820A (en) * 1994-11-15 1999-11-30 Kleindiek; Stephan Electromechanical positioning unit
US20060138897A1 (en) * 2003-07-04 2006-06-29 Peter Hess Tool head comprising piezoelectric actuators

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
Clévy et al. (A micromanipulation cell including a tool changer, J. Micromech. Microeng. 15(2005) S292-S301). *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US10525207B2 (en) 2010-07-22 2020-01-07 Becton, Dickinson And Company Dual chamber syringe with retractable needle

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DE112006004191A5 (de) 2009-10-01
ATE537920T1 (de) 2012-01-15
EP2086701A1 (de) 2009-08-12
WO2008052494A1 (de) 2008-05-08
EP2086701B1 (de) 2011-12-21

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