US3547713A - Methods of making structural materials having a low temperature coefficient of the modulus of elasticity - Google Patents

Methods of making structural materials having a low temperature coefficient of the modulus of elasticity Download PDF

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US3547713A
US3547713A US631686A US3547713DA US3547713A US 3547713 A US3547713 A US 3547713A US 631686 A US631686 A US 631686A US 3547713D A US3547713D A US 3547713DA US 3547713 A US3547713 A US 3547713A
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temperature
modulus
materials
elasticity
temperature coefficient
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Samuel Steinemann
Martin Peter
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Institut Straumann AG
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Institut Straumann AG
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/12—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials
    • H01F1/14—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of soft-magnetic materials metals or alloys
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C27/00—Alloys based on rhenium or a refractory metal not mentioned in groups C22C14/00 or C22C16/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C28/00—Alloys based on a metal not provided for in groups C22C5/00 - C22C27/00
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • G—PHYSICS
    • G04—HOROLOGY
    • G04B—MECHANICALLY-DRIVEN CLOCKS OR WATCHES; MECHANICAL PARTS OF CLOCKS OR WATCHES IN GENERAL; TIME PIECES USING THE POSITION OF THE SUN, MOON OR STARS
    • G04B17/00—Mechanisms for stabilising frequency
    • G04B17/20—Compensation of mechanisms for stabilising frequency
    • G04B17/22—Compensation of mechanisms for stabilising frequency for the effect of variations of temperature
    • G04B17/227—Compensation of mechanisms for stabilising frequency for the effect of variations of temperature composition and manufacture of the material used
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/0302—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity characterised by unspecified or heterogeneous hardness or specially adapted for magnetic hardness transitions
    • H01F1/0306—Metals or alloys, e.g. LAVES phase alloys of the MgCu2-type

Definitions

  • the components of the material are selected in type and quantity such that the material exhibits an atomic, paramagnetic susceptibility x 50-10- emE/g.-atom at room temperature and a negative temperature coefficient of the susceptibility d /a'T.
  • the components are melted together, and a preferred orientation of the crystals by at least a mechanical or a thermal treatment of the material is produced.
  • the present invention relates to methods of making structural materials and elements having a low temperature coeflicient of the modulus of elasticity and more particularly having such coeflicient varying only slightly around zero.
  • moduli namely the modulus of elasticity (for example in the bending of tuning forks, spiral springs etc), the shear modulus (under torsion, for example, in spirally wound tension springs) or the compression modulus, as well as combinations of all of these moduli.
  • the known structural materials which exhibit suitably small and adaptable temperature coefficients are based upon ferromagnetic processes.
  • these materials under the influence of external load, there is a change in the local direction of the spontaneous magnetization in such a manner that the magnetostrictive distortion caused by the change in magnetization increases the shape changing effect of the load on the body (this is known as magnetostrictive extension under tension and conversely, according to the direction of stress).
  • magnetostrictive extension under tension this is known as magnetostrictive extension under tension and conversely, according to the direction of stress.
  • the A E effect is particularly strong in the pure metals Ni, Co, Fe and is brought about essentially by the linear magnetostriction effect and is practically suppressed by external magnetic fields or cold working (both of which disturb the free inception of the spontaneous magnetization in the domains). If, on the other hand, the volume magnetostriction effect is preponderant, as for example for certain Fe-Ni, Fe-Ni-Co and Fe-Co-Cr alloys and others, then the anomalous behaviour in the ferromagnetic temperature region does not completely vanish even under conditions of magnetic saturation or intense cold working.
  • the present invention relates to a method of producing structural materials, of the elinvar type having a small temperature coefficient of the elastic moduli, which are sensibly temperature independent.
  • the method uses a paramagnetic material with an atomic susceptibility x 50-10 emE/g.-atom at room temperature and a negative temperature-coeflicient of this susceptibility, e.g. d /dT, and wherein a texture is produced by mechanical or heat processing. This texture is related to the type and orientation of the stress in the structural element.
  • the overall composition, or that of principal phase of the material has an electron concentration e/ a comprised in e/ a equal to 2.5-3.7 or 4.1-5.7 or 6.1-7.8 or
  • the electron concentration e/a is the ratio of the mean number of electrons situated externally of closed shells, that is to say the electrons determining bonding, to the number of atoms.
  • n elements with the percentages by weight g,, the atomic weights A, and the number 1/, of electrons outside the closed shells (valencies) the atomic percentages are calculated by and the electron concentrations are given by e 1 11 run
  • the mechanical or heat processing used to produce the texture may be drawing, or rolling or recrystallization annealing.
  • the texture is characterised by the product-sum I of the direction-cosine between the crystal-orientation and the stress direction in the structural element, taken as the mean over all crystallite orientations in the material.
  • the product-sum i is given by the expression in the case of cubic materials.
  • I 0.2 for the elasticity modulus, and I 0.2 for the shear modulus (stress axis torsion axis).
  • hexagonal materials I O.25 for the elasticity modulus and I O.25 for the shear modulus.
  • the cohesion energy of a metal is comprised additively of various contributions. Essentially there are three components of the energy to be considered, which originate from the interaction between the ions of the crystal lattice, between the ions and free electrons and between the free or itinerant electrons themselves. The first two components are responsible for definite uniform characteristics of the elastic behaviour of the single crystal; on the other hand the last component is decisive for certain metals and alloys, in particular in respect of the temperature relationship of the elasticity (usually this component due to the electron gas is small or independent of temperature). Upon these effects depends a group of materials of this invention, principally metals and alloys but under certain circumstances also semiconductors. These materials are not ferromagnetic and satisfy also the further requirements of resistance against corrosion, easy workability, small mechanical losses, mechanical strength and so on.
  • the high density of states fi(E is characterised by high paramagnetic susceptibility high specific heat of the electrons, and frequently also by a high superconductivity transition temperature.
  • the temperature relationship with KLE is most clearly seen from the temperature behaviour of )4 namely d /dT.
  • FIGS. la-lc in which there are represented, for the transition element of the third, fourth and fifth periods, and their alloys, the paramagnetic susceptibility (FIG. 1a), the temperature coefficient thereof ld dT (FIG. 1b) and the temperature coefficient of the elasticity modulus (FIG. 10), plotted in each case With respect to the electron concentration e/a.
  • the electron concentration e/a embraces completely all alloys with two or more components between the elements of different groups and periods of the period system.
  • thermocompensating alloys With structural materials fulfilling the requirements of the invention, the contribution of the free electrons to the elastic energy results in an anomalous temperature relationship with the elasticity. These effects are however contrasted with the conventional anomalous behaviour.
  • the temperature independence of the previously known thermocompensating alloys is always limited at an upper temperature, in fact at that point where the required homomorphous transformations vanish; the reversible transformation of ferromagnetism to paramagnetism is the most well-known example; this anomaly extends up to the Curie temperature.
  • FIGS. 1a to 10 depict isotropic structures.
  • FIGS. 2a to 2] illustrates the dependence of orientation with temperature.
  • FIG. 3 depicts a pole figure for the cubic case.
  • FIG. 4 illustrates the crystal structures of the elements and the approximate phase structure of the binary alloy series of the transition elements.
  • FIGS. la to 10, in particular 10, refer to isotropic structures, e.g., all crystal orientations are equally prohable.
  • the behaviour of these materials is an anisotropic property of the crystal which has to be taken in account for the technical use in two ways; it can either be provided a texture by suitable mechanical or heat processing, or the preferred orientation in the material as obtained with customary processing is examined (for example with X-ray methods) and oriented against the stress direction in the structural element. These orientations are fully described by the product-sum 5.
  • Structural materials according to this invention should not only retain their rigidity with varying temperature, its technical application needs also sufficient mechanical strength which can be obtained through different forms of hardening processes.
  • Polycrystalline solid bodies may have, as is known, numerous anisotropic characteristics which originate from the texture (see the textbook by G. Wassermann and Johanna Grewen Texturen metallischer Werkstoffe, Springer Verlag, Berlin, Gottingen, Heidelberg, 1962). It is however less frequently investigated how the temperature coefficients of the elasticity modulus can depend upon a texture.
  • the AE effect of nickel is strongly anisotropic because the shape magnetostriction is strongly anisotropic; in the classical alloys having a small temperature coeflicient of the E modulus, which are known under the marks Nivarox, Ni-Span C, etc., where the volume magnetostriction predominates, the direction dependence is, on the contrary, small and in practice is not considered or controlled.
  • the materials in accordance with the invention depend clearly upon single crystal properties, whose anisoptropic properties cannot be ignored or neglected.
  • the elasticity theory describes the strains in the me chanically stressed single crystal by means of elastic constants.
  • cubic crystal which in the following will be taken as an example, it will suffice to consider three quantities, c and e (0 corresponds to ex tension along a main axis in which also the force is effective, C is an extension normal to this main axis and to the direction of the force, C44 is a shear in planes of two main axes).
  • C and e corresponds to ex tension along a main axis in which also the force is effective
  • C is an extension normal to this main axis and to the direction of the force
  • C44 is a shear in planes of two main axes.
  • g is negative for i 0.09 and e is negative for I 0.32. It appears to be quite certain therefore that, as regards the technical utilisation of the materials in accordance with the invention, this direction dependence is to be taken into account, and in fact for obtaining uniform results a definite texture, that is to say a more or less rigidly determined value of I is to be imposed upon the structural element of sensibly constant elasticity. A definite I is therefore necessary and is also a means in accordance with the invention for adjusting the temperature coefilcients of the elastic moduli.
  • An isotropic polycrystalline structure (whose I would be 0.2) can frequently not be obtained through processing and it is a better procedure to produce a texture with suitable processing steps; according to this invention, this texture is then to orient with regard to the appearing stress in the structural element, e.g. the texture is produced with regard to the given type and direction of stress or the structural element is cut in suitable orientation from the textured material.
  • the decisive quantity for the texture relationship is in any case the quantity I taken as the mean over the polycrystalline material; P can be represented in a so-called pole figure,
  • a texture can be achieved by drawing and/or rolling at room or elevated temperatures; recristallization annealing is also a process to create or sharpen a texture.
  • the conditions are frequently such that, for example, in cubic body-centered materials (pure metals, alloys behave frequently otherwise) the 110 direction lies parallel to the drawing or rolling direction I against this working direction), and for cubic facecentered materials a portion of the crystallites adjusts its 100 direction and another part its 111 direction parallel to the drawing or rolling direction (against the working direction, 1 has then values between near 0 and 0.33).
  • FIG. 4 there are set out the crystal structures of the elements and the approximate phase structure of the binary alloy series of the transition metals.
  • the comparison with FIG. 1 now shows the previously stated fact that the materials in accordance with the invention are not restricted to a fixed crystal structure.
  • such materials in accordance with the invention are consistent also with complex structures if the condition is fulfilled that I ⁇ (E is large and that TABLE 1 40 atom percent Ir 60 atom percent- Nb 67 atom percent. Re 33 atom percent. W 67 atom percent- R11 33 atom percent Ca 1-phaso. ⁇ Of structural type wMn. ⁇ Of structural type 015 (Laves phase).
  • Cooperative processes of the electrons characterise magnetic phenomena.
  • magnetic phenomena suffer strong perturbation by cold work or external fields; the classical ferromagnetic alloys with constant elastic modulus show in fact a marked decrease of the temperature coeificient when cold worked or exposed to a magnetic field.
  • Such influences are absent in materials according to the invention.
  • a high density of states fi(E signifies in fact that geometrical and chemical perturbations of the perfectly regular lattice, e.g. lattice faults and interstitial impurity atoms, are well screened off (substitutional atoms, either impurities or alloying additions are considered as bonding components), while at the same time the reciprocal forces between the faults diminish.
  • Alloy systems of structural materials according to this inventions and which shall be capable of polyphase hardening, precipitation hardening or dispersion hardening, have an electron concentration e/a where at least the main phase lies in the previously given ranges.
  • These hardening mechanisms involve different phases or a phase decomposition. The properties of the whole depend then on the proportions of present phases, which themselves have different e/a-values and hence also different thermoelastic properties. Resulting from the inconsistency, there now appears a basically different behaviour of paramagnetic alloys. As is evident from FIG. 1c, very small temperature coefficients alternate with strongly negative coefficients of temperature within very closely adjacent e/a ranges.
  • the temperature coefficient is adjustable through a different annealing heat treatment.
  • An example of this is the hardenable alloy system 25% zirconium and 75% niobium, which when rapidly cooled down from, for example, 1000 C., can then be cold formed about by drawing (whereby a 110 drawn texture results), whereafter a heat treatment at SSW-600 for four hours brings the required properties.
  • the temperature coefficient is positive, but with the phase separation, the zirconium rich mixed crystal separates which has a markedly negative temperature coefficient, separates out and makes the temperature coetficient of the whole more negative and towards zero.
  • the electron concentration e/ a of this alloy amounts to 4.75.
  • a material in accordance with the invention of given electron concentration is heat treated above the temperature dependent solubility limit (Solvus) and quenched, and then (possibly after cold forming) heat treated below the solubility limit. Due to the displacement of e/a in the matrix and the contribution of the precipitate, the adjustment of the temperature coefiicient is achieved. Addition elements whereby the precipitation hardening can be achieved without an excessive degree of solubility usually follow definite laws, known as the Hume-Rothery Laws.
  • An example is an alloy of Nb and 5% Cr which has an e/a value of 5.1 and which can be subjected to a similar treatment to that above described for the Nb Zr alloy.
  • the precipitated phase effecting the hardening is NbCr
  • Such alloys are suitable for use in tuned measuring devices, for example clocks and in fact for its elastic elements in the form of spiral springs, tuning forks or other forms of vibratory element.
  • electromechanical filters may be made from such alloys.
  • Spring elements which have such small thermoelastic coefficients are employed also for force measurement, for example in balances, electrical measuring instruments, levelling apparatus and similar devices.
  • Another application of such alloys is for structural materials capable of retaining their rigidity over a wide temperature range; such needs are for example present in turbines, planes, or rockets where components are subjected to mechanical stresses and whose elasticity shall not vary with temperature or where stresses might induce oscillations which should be controllable over a wide temperature range.
  • a method of producing an elastically stressed body of a non-magnetic elinvar which comprises:
  • a method as claimed in claim 1 including the step of producing a preferred orientation by drawing or rolling, and recrystallization annealing in the temperature region of homogeneous equilibrium phase structure.
  • temperaure coefficient is adjusted, sai-d adjustment including steps of a heat treatment above the equilibrium decomposition temperature and quenching, followed by a heat treatment below the decomposition temperature.

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US631686A 1966-04-22 1967-04-18 Methods of making structural materials having a low temperature coefficient of the modulus of elasticity Expired - Lifetime US3547713A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3798077A (en) * 1971-09-24 1974-03-19 Siemens Ag Method for aligning mechanical filters
US3974001A (en) * 1966-04-22 1976-08-10 Institut Dr. Ing. Reinhard Straumann, A.G. Paramagnetic alloy
US4089711A (en) * 1976-04-03 1978-05-16 The Research Institute For Iron, Steel And Other Metals Of The Tohoku University Antiferromagnetic chromium base invar-type alloys and a method of producing the same
US5881026A (en) * 1997-06-20 1999-03-09 Montres Rolex S.A. Self-compensating balance spring for a mechanical oscillator of a balance-spring/balance assembly of a watch movement and process for manufacturing this balance-spring
US6329066B1 (en) * 2000-03-24 2001-12-11 Montres Rolex S.A. Self-compensating spiral for a spiral balance-wheel in watchwork and process for treating this spiral
US20060225526A1 (en) * 2002-07-12 2006-10-12 Gideon Levingston Mechanical oscillator system
US20070140065A1 (en) * 2003-10-20 2007-06-21 Gideon Levingston Balance wheel, balance spring and other components and assemblies for a mechanical oscillator system and methods of manufacture
US20090116343A1 (en) * 2005-05-14 2009-05-07 Gideon Levingston Balance spring, regulated balance wheel assembly and methods of manufacture thereof
US20100034057A1 (en) * 2006-09-08 2010-02-11 Gideon Levingston Thermally compensating balance wheel
EP3663867A1 (de) * 2018-12-05 2020-06-10 Cartier International AG Kompensierende spiralfeder für eine uhr oder grossuhr aus einer niob-molybdän-legierung

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CH527412A (de) * 1970-07-17 1972-08-31 Straumann Inst Ag Spannband für die Spannbandaufhängung eines drehbaren Messwerks
EP1258786B1 (de) 2001-05-18 2008-02-20 Rolex Sa Selbstkompensierende Feder für einen mechanischen Oszillator vom Unruh-Spiralfeder-Typ

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3167692A (en) * 1961-04-24 1965-01-26 Bell Telephone Labor Inc Superconducting device consisting of a niobium-titanium composition
US3215569A (en) * 1962-02-09 1965-11-02 Jr George D Kneip Method for increasing the critical current of superconducting alloys
US3253191A (en) * 1961-10-11 1966-05-24 Bell Telephone Labor Inc Nb-zr superconductor and process of making the same
US3271200A (en) * 1962-06-19 1966-09-06 Metallgesellschaft Ag Process for the production of superconductive wires and bands
US3275480A (en) * 1962-08-27 1966-09-27 Jr Jesse O Betterton Method for increasing the critical current density of hard superconducting alloys and the improved products thereof
US3374123A (en) * 1964-03-04 1968-03-19 Foundation Method of manufacturing non-magnetic, elastic articles having a small change of vibration and deflection for temperature change

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3167692A (en) * 1961-04-24 1965-01-26 Bell Telephone Labor Inc Superconducting device consisting of a niobium-titanium composition
US3253191A (en) * 1961-10-11 1966-05-24 Bell Telephone Labor Inc Nb-zr superconductor and process of making the same
US3215569A (en) * 1962-02-09 1965-11-02 Jr George D Kneip Method for increasing the critical current of superconducting alloys
US3271200A (en) * 1962-06-19 1966-09-06 Metallgesellschaft Ag Process for the production of superconductive wires and bands
US3275480A (en) * 1962-08-27 1966-09-27 Jr Jesse O Betterton Method for increasing the critical current density of hard superconducting alloys and the improved products thereof
US3374123A (en) * 1964-03-04 1968-03-19 Foundation Method of manufacturing non-magnetic, elastic articles having a small change of vibration and deflection for temperature change

Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3974001A (en) * 1966-04-22 1976-08-10 Institut Dr. Ing. Reinhard Straumann, A.G. Paramagnetic alloy
US3798077A (en) * 1971-09-24 1974-03-19 Siemens Ag Method for aligning mechanical filters
US4089711A (en) * 1976-04-03 1978-05-16 The Research Institute For Iron, Steel And Other Metals Of The Tohoku University Antiferromagnetic chromium base invar-type alloys and a method of producing the same
KR100725400B1 (ko) * 1997-06-20 2007-12-27 로렉스 소시에떼아노님 시계용 무브먼트의 밸런스 스프링/밸런스 조립체의 기계 오실레이터용 자기보정 밸런스 스프링과, 이 밸런스 스프링의 제조방법
US5881026A (en) * 1997-06-20 1999-03-09 Montres Rolex S.A. Self-compensating balance spring for a mechanical oscillator of a balance-spring/balance assembly of a watch movement and process for manufacturing this balance-spring
US6503341B2 (en) 1999-03-26 2003-01-07 Montres Rolex S.A. Self-compensating spiral for a spiral balance-wheel in watchwork and process for treating this spiral
US6329066B1 (en) * 2000-03-24 2001-12-11 Montres Rolex S.A. Self-compensating spiral for a spiral balance-wheel in watchwork and process for treating this spiral
US20060225526A1 (en) * 2002-07-12 2006-10-12 Gideon Levingston Mechanical oscillator system
US7641381B2 (en) * 2002-07-12 2010-01-05 Gideon Levingston Mechanical oscillator system
US20070140065A1 (en) * 2003-10-20 2007-06-21 Gideon Levingston Balance wheel, balance spring and other components and assemblies for a mechanical oscillator system and methods of manufacture
US7726872B2 (en) 2003-10-20 2010-06-01 Gideon Levingston Balance wheel, balance spring and other components and assemblies for a mechanical oscillator system and methods of manufacture
US20090116343A1 (en) * 2005-05-14 2009-05-07 Gideon Levingston Balance spring, regulated balance wheel assembly and methods of manufacture thereof
US8333501B2 (en) 2005-05-14 2012-12-18 Carbontime Limited Balance spring, regulated balance wheel assembly and methods of manufacture thereof
US20100034057A1 (en) * 2006-09-08 2010-02-11 Gideon Levingston Thermally compensating balance wheel
US8100579B2 (en) 2006-09-08 2012-01-24 Gideon Levingston Thermally compensating balance wheel
EP3663867A1 (de) * 2018-12-05 2020-06-10 Cartier International AG Kompensierende spiralfeder für eine uhr oder grossuhr aus einer niob-molybdän-legierung

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CH587866A4 (de) 1970-02-13
CH557557A (de) 1974-12-31
DE1558513A1 (de) 1972-02-17
GB1183476A (en) 1970-03-04
DE1558513C3 (de) 1974-04-04
NL6705413A (de) 1967-10-23
DE1558513B2 (de) 1973-08-30

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