EP3502785B1 - Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication - Google Patents

Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication Download PDF

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Publication number
EP3502785B1
EP3502785B1 EP17209682.8A EP17209682A EP3502785B1 EP 3502785 B1 EP3502785 B1 EP 3502785B1 EP 17209682 A EP17209682 A EP 17209682A EP 3502785 B1 EP3502785 B1 EP 3502785B1
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EP
European Patent Office
Prior art keywords
titanium
niobium
alloy
deformation
equal
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EP17209682.8A
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German (de)
English (en)
French (fr)
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EP3502785A1 (fr
Inventor
Christian Charbon
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Nivarox Far SA
Nivarox SA
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Nivarox Far SA
Nivarox SA
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Application filed by Nivarox Far SA, Nivarox SA filed Critical Nivarox Far SA
Priority to EP17209682.8A priority Critical patent/EP3502785B1/fr
Priority to US16/143,764 priority patent/US11586146B2/en
Priority to JP2018204827A priority patent/JP6764915B2/ja
Priority to CN201811412811.7A priority patent/CN109946945B/zh
Priority to RU2018144937A priority patent/RU2696327C1/ru
Publication of EP3502785A1 publication Critical patent/EP3502785A1/fr
Priority to JP2020130704A priority patent/JP2020187134A/ja
Publication of EP3502785B1 publication Critical patent/EP3502785B1/fr
Application granted granted Critical
Priority to US18/060,228 priority patent/US11966198B2/en
Priority to JP2023175743A priority patent/JP2024016031A/ja
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Classifications

    • 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
    • G04B17/04—Oscillators acting by spring tension
    • G04B17/06—Oscillators with hairsprings, e.g. balance
    • G04B17/066—Manufacture of the spiral spring
    • 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
    • C22C27/02—Alloys based on vanadium, niobium, or tantalum
    • 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
    • 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
    • C22F1/16—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of other metals or alloys based thereon
    • C22F1/18—High-melting or refractory metals or alloys based thereon
    • 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
    • G04B17/04—Oscillators acting by spring tension
    • G04B17/06—Oscillators with hairsprings, e.g. balance
    • 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

Definitions

  • the invention relates to a spiral spring intended to equip a balance of a clockwork movement, as well as to a method of manufacturing such a spiral spring.
  • spiral springs are also centered on the concern for thermal compensation, so as to guarantee regular chronometric performance. This requires obtaining a thermoelastic coefficient close to zero. We are also looking to produce spiral springs exhibiting limited sensitivity to magnetic fields.
  • the document WO 2005/045532 in the name of Seiko describes a clock spring for ensuring high precision and stable operation of precision mechanisms such as clocks, which can be a clock spring, a mainspring, or a balance spring.
  • This spring is formed of a special titanium alloy and has an S-shape when it is freely deployed, in which the inflection point at which the direction of curvature of the freely deployed form changes is formed more inside than the middle of an inner end to the winding side end and from an outer end to the opposite end to the inner end.
  • the titanium alloy has a high tensile stress and a low average Young's modulus, making it possible to increase the mechanical energy stored in the mainspring.
  • This alloy may be a titanium alloy with an element from the vanadium group, with in particular a proportion by weight of element from the vanadium group of 20 to 80%, and more particularly of 30 to 60%.
  • the mass proportion of constituents other than titanium can exceed 50%.
  • no more precise composition of the alloy is disclosed for the spring described.
  • the document WO2015 / 189278 in the name of Cartier describes a spiral spring in a titanium alloy containing: a titanium base, from 10 to 40 atomic% of at least one element among Nb, Ta or V, from 0 to 3 atomic% of oxygen, 0 to 6 atomic% zirconium; and from 0 to 5 atomic% hafnium.
  • This hairspring is less sensitive to temperature, and has a lower density than a conventional hairspring.
  • the document WO2018 / 172164 in the name of the University of Lorraine describes a metastable ⁇ titanium alloy comprising, in mass percentage, between 24 and 45% niobium, between 0 and 20% of zirconium, between 0 and 10% of tantalum and / or between 0 and 1.5% silicon and / or less than 2% oxygen.
  • This alloy has a crystallographic structure which comprises a mixture of austenitic phase and alpha phase, and the presence of omega phase precipitates, the volume fraction of which is less than 10%.
  • This document also describes a clockwork spring made from such an alloy, and a method of manufacturing such a spring.
  • the document EP2993531 in the name of Précision Engineering AG describes a method of shaping a mechanical spring, in particular a spiral spring, comprising the steps of preparing a spring, in particular a spiral spring, comprising at least one curved section intended for reshaping with at least one deformable section, then performing a local heating step of at least the deformable section to a first temperature, which is within a semi-hot formation temperature range of the material of the deformable section , then in imparting a movement of the deformable section to obtain a predetermined shape of a curve in the deformable section, this movement being carried out either after or during the heating step and in a semi-hot state, or else before the heating step.
  • a press bulletin H. Moser & Cie and Précision Engineering dated 11/22/2016 describes a balance spring for a watch regulating organ in niobium-titanium alloy, the composition of which is not disclosed.
  • the invention proposes to define a new type of spiral spring intended to equip a balance of a clockwork movement, based on the selection of a particular material, and to develop the appropriate manufacturing process.
  • the spiral spring according to the invention is made of a niobium-based alloy having an essentially single-phase structure, is paramagnetic and has the mechanical properties and the thermoelastic coefficient required for its use as a spiral spring for a balance. It is obtained using a manufacturing process that is simple to implement, allowing easy shaping and adjustment of the thermal compensation, in a few steps.
  • the invention relates to a spiral spring intended to equip a balance of a clockwork movement and produced in a binary type alloy comprising niobium and titanium.
  • the spiral spring according to the invention is made from an NbTi alloy having an essentially single-phase structure in the form of a solid ⁇ -Nb-Ti solution, the titanium content in the ⁇ form being less than or equal to 10% by volume.
  • the titanium content in ⁇ form is preferably less than or equal to 5% by volume, and more preferably less than or equal to 2.5% by volume.
  • the alloy used in the present invention comprises between 44% and 49% by weight of titanium, preferably between 46% and 48% by weight of titanium, and preferably said alloy comprises more than 46.5% by weight. weight of titanium and said alloy comprises less than 47.5% by weight of titanium.
  • the titanium content is greater than or equal to 46.5% by weight relative to the total of the composition.
  • the titanium content is less than or equal to 47.5% by weight relative to the total of the composition.
  • the NbTi alloy used in the present invention does not comprise other elements except for possible and inevitable traces. This prevents the formation of fragile phases.
  • the oxygen content is less than or equal to 0.10% by weight of the total, or even less than or equal to 0.085% by weight of the total.
  • the tantalum content is less than or equal to 0.10% by weight of the total.
  • the carbon content is less than or equal to 0.04% by weight of the total, in particular less than or equal to 0.020% by weight of the total, or even less than or equal to 0.0175% by weight of the total.
  • the iron content is less than or equal to 0.03% by weight of the total, in particular less than or equal to 0.025% by weight of the total, or even less than or equal to 0.020% by weight of the total.
  • the nitrogen content is less than or equal to 0.02% by weight of the total, in particular less than or equal to 0.015% by weight of the total, or even less than or equal to 0.0075% by weight of the total.
  • the hydrogen content is less than or equal to 0.01% by weight of the total, in particular less than or equal to 0.0035% by weight of the total, or even less than or equal to 0.0005% by weight of the total.
  • the silicon content is less than or equal to 0.01% by weight of the total.
  • the nickel content is less than or equal to 0.01% by weight of the total, in particular less than or equal to 0.16% by weight of the total.
  • the content of ductile material, such as copper, in the alloy is less than or equal to 0.01% by weight of the total, in particular less than or equal to 0.005% by weight of the total.
  • the aluminum content is less than or equal to 0.01% by weight of the total.
  • the spiral spring of the invention has an elastic limit greater than or equal to 600 MPa.
  • this spiral spring has an elastic modulus less than or equal to 100 GPa, and preferably between 60 GPa and 80 GPa.
  • the spiral spring according to the invention has a thermoelastic coefficient, also called CTE, allowing it to guarantee the maintenance of chronometric performance despite the variation in the temperatures of use of a watch incorporating such a spiral spring.
  • the CTE of the alloy must be close to zero ( ⁇ 10 ppm / ° C) to obtain a thermal coefficient of the oscillator equal to ⁇ 0.6 s / d / ° C.
  • E is the Young's modulus of the hairspring, and, in this formula, E, ⁇ and ⁇ are expressed in ° C -1 .
  • CT is the thermal coefficient of the oscillator
  • (1 / E. DE / dT) is the CTE of the balance spring alloy
  • ⁇ is the expansion coefficient of the balance and ⁇ that of the balance spring.
  • the quenching step ⁇ is a solution treatment, with a duration of between 5 minutes and 2 hours at a temperature of between 700 ° C and 1000 ° C, under vacuum, followed by cooling under gas .
  • this beta quenching is a treatment for dissolving, between 5 minutes and 1 hour at 800 ° C. under vacuum, followed by cooling under gas.
  • the heat treatment is carried out for a period of between 1 hour and 15 hours at a temperature of between 350 ° C and 700 ° C. More preferably, the heat treatment is carried out for a period of between 5 hours and 10 hours at a temperature of between 350 ° C and 600 ° C. Even more preferably, the heat treatment is carried out for a period of between 3 hours and 6 hours at a temperature of between 400 ° C and 500 ° C.
  • a deformation step generally refers to one or more deformation treatments, which may include drawing and / or rolling.
  • Wire drawing may require the use of one or more dies during the same deformation step or during different deformation steps if necessary.
  • Wire drawing is carried out until a wire of round section is obtained.
  • Rolling can be carried out in the same deformation step as wire drawing or in another subsequent deformation step.
  • the last deformation treatment applied to the alloy is rolling, preferably with a rectangular profile compatible with the entry section of a stranding spindle.
  • the total strain rate is between 1 and 5, preferably between 2 and 5.
  • This strain rate corresponds to the classic formula 2ln (d0 / d), where d0 is the diameter of the last beta hardening, and where d is the diameter of the hardened wire.
  • a blank is used, the dimensions of which are as close as possible to the desired final dimensions so as to limit the number of heat treatment and deformation steps and to maintain an essentially single-phase structure ⁇ of the NbTi alloy.
  • the final structure of the NbTi alloy of the spiral spring may be different from the initial structure of the blank, for example the titanium content in ⁇ form may have varied, the main thing being that the final structure of the NbTi alloy of the spiral spring is essentially single-phase, the titanium of the niobium-based alloy being essentially in the form of a solid solution with the niobium in the ⁇ phase , the titanium content in the ⁇ phase being less than or equal to 10% by volume, preferably less than or equal to 5% by volume, more preferably less than or equal to 2.5% by volume.
  • the titanium content in the ⁇ phase is preferably less than or equal to 5% by volume, more preferably less than or equal to 2.5% by volume, or even close to
  • the method of the invention comprises a single deformation step with a deformation rate between 1 and 5, preferably between 2 and 5.
  • the deformation rate corresponds to the conventional formula 2ln (d0 / d) , where d0 is the diameter of the last beta hardening or that of a straining step, and d is the diameter of the hardened wire obtained in the following straining step.
  • a particularly preferred method of the invention comprises, after the quenching step ⁇ , a deformation step including wire drawing by means of several dies then rolling, a stranding step then a final heat treatment step (called fixing).
  • the method of the invention can further comprise at least one intermediate heat treatment step, so that the method comprises for example after the hardening step ⁇ , a first deformation step, an intermediate heat treatment step, a second deformation step, the scaling step then a final heat treatment step.
  • the total deformation rate obtained after several deformation steps, and preferably by a single deformation step, the number of heat treatments as well as the parameters of the heat treatments are chosen to obtain a spiral spring exhibiting a thermoelastic coefficient as close as possible to 0.
  • the method of the invention further comprises, before the deformation step, and more particularly before the wire drawing, a step of depositing, on the alloy blank, a surface layer of a ductile material chosen from the group comprising copper, nickel, cupro-nickel, cupro-manganese, gold, silver, nickel-phosphorus Ni-P and nickel-boron Ni-B, to facilitate the formatting as a wire.
  • a ductile material chosen from the group comprising copper, nickel, cupro-nickel, cupro-manganese, gold, silver, nickel-phosphorus Ni-P and nickel-boron Ni-B, to facilitate the formatting as a wire.
  • the ductile material preferably copper, is thus deposited at a given moment to facilitate the shaping of the wire by drawing and drawing, so that there remains a thickness preferably between 1 and 500 micrometers on the wire has a total diameter of 0.2 to 1 millimeter.
  • the supply of ductile material in particular copper, can be galvanic, PVD or CVD, or else mechanical, it is then a jacket or a tube of ductile material such as copper which is fitted to a bar of niobium alloy. titanium to a large diameter, then which is thinned during the step (s) of deformation of the composite bar.
  • the thickness of the layer of ductile material deposited is chosen so that the ratio of the area of ductile material / area of NbTi for a given section of wire is less than 1, preferably less than 0.5, and more preferably between 0.01 and 0.4.
  • Such a thickness of ductile material, and in particular copper, makes it possible to easily roll the Cu / NbTi composite material.
  • the method of the invention can comprise, after the deformation step, a step of removing said surface layer of ductile material.
  • the ductile material is removed once all the deformation treatment operations have been carried out, that is to say after the last rolling, before the stretching.
  • the wire is freed from its layer of ductile material, such as copper, in particular by chemical attack, with a solution based on cyanides or based on acids, for example nitric acid.
  • the surface layer of ductile material is kept on the spiral spring, the thermoelastic coefficient of the niobium-based alloy being adapted accordingly so as to compensate for the effect of the ductile material.
  • the thermoelastic coefficient of the niobium-based alloy can be easily adjusted by choosing the appropriate strain rate and heat treatments.
  • the surface layer of ductile material retained makes it possible to obtain a perfectly regular final wire section.
  • the ductile material can here be copper or gold, deposited by galvanic route, PVD or CVD.
  • the method of the invention may further comprise a step of depositing, on the surface layer of preserved ductile material, a final layer of a material chosen from the group comprising Al 2 O 3 , TiO 2 , SiO 2 and AlO , by PVD or CVD. It is also possible to provide a final gold layer deposited by galvanic gold flash if the gold has not already been used as a ductile material for the surface layer. You can also use copper, nickel, cupro-nickel, cupro-manganese, silver, nickel-phosphorus Ni-P and nickel-boron Ni-B for the final layer, as long as the material of the final layer is different from the ductile material of the surface layer.
  • This final layer has a thickness of 0.1 ⁇ m to 1 ⁇ m and makes it possible to color the hairspring or to obtain insensitivity to climatic aging (temperature and humidity).
  • the invention thus makes it possible to produce a spiral spring for a balance in a niobium-titanium type alloy, typically containing 47% by weight of titanium (40-49%).
  • a niobium-titanium type alloy typically containing 47% by weight of titanium (40-49%).
  • By a limited number of deformation and heat treatment steps it is possible to obtain an essentially single-phase microstructure of ⁇ -Nb-Ti in which the titanium is in the ⁇ form.
  • This alloy has high mechanical properties, by combining a very high elastic limit, greater than 600 MPa, and a very low modulus of elasticity, of the order of 60 Gpa to 80 GPa. This combination of properties is well suited for a spiral spring.
  • Such an alloy is known and used for the manufacture of superconductors, such as magnetic resonance imaging devices, or particle accelerators, but is not used in watchmaking.
  • a binary type alloy comprising niobium and titanium, of the type selected above for the implementation of the invention also exhibits an effect similar to that of “Elinvar”, with a thermoelastic coefficient practically zero. within the temperature range of usual use of watches, and suitable for the manufacture of self-compensating balance springs.
  • such an alloy is paramagnetic.
  • such an alloy makes it possible to manufacture a spiral spring according to a simple manufacturing process, comprising few steps, allowing easy shaping and adjustment of the thermal compensation.
  • this niobium-titanium type alloy can easily be covered with a ductile material, such as copper, which greatly facilitates its deformation by drawing.
  • a ductile material such as copper
  • a hairspring was manufactured according to the process of the invention from a wire of given diameter made of a niobium-based alloy consisting of 53% by weight of niobium and 47% by weight of titanium and having undergone a quenching step.
  • ⁇ type so that the titanium is essentially in the form of a solid solution with the niobium in the ⁇ phase.
  • the wire undergoes a first deformation step (wire drawing), an intermediate heat treatment step, a second deformation step (drawing and rolling), the stretching step then the last treatment step thermal corresponding to the fixing of the hairspring.
  • the hairspring is associated with a cupro-beryllium balance and the thermal coefficient CT of the oscillator thus obtained is measured.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Physics & Mathematics (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Thermal Sciences (AREA)
  • General Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Springs (AREA)
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EP17209682.8A 2017-12-21 2017-12-21 Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication Active EP3502785B1 (fr)

Priority Applications (8)

Application Number Priority Date Filing Date Title
EP17209682.8A EP3502785B1 (fr) 2017-12-21 2017-12-21 Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication
US16/143,764 US11586146B2 (en) 2017-12-21 2018-09-27 Spiral spring for clock or watch movement and method of manufacture thereof
JP2018204827A JP6764915B2 (ja) 2017-12-21 2018-10-31 固定式時計又は携行式時計のムーブメントのための渦巻き状のばね及びその製造方法
CN201811412811.7A CN109946945B (zh) 2017-12-21 2018-11-23 用于钟表机芯的螺旋弹簧及其制造方法
RU2018144937A RU2696327C1 (ru) 2017-12-21 2018-12-18 Спиральная пружина для механизма часов, в частности наручных, и способ ее изготовления
JP2020130704A JP2020187134A (ja) 2017-12-21 2020-07-31 固定式時計又は携行式時計のムーブメントのための渦巻き状のばね及びその製造方法
US18/060,228 US11966198B2 (en) 2017-12-21 2022-11-30 Spiral spring for clock or watch movement and method of manufacture thereof
JP2023175743A JP2024016031A (ja) 2017-12-21 2023-10-11 固定式時計又は携行式時計のムーブメントのための渦巻き状のばね及びその製造方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP17209682.8A EP3502785B1 (fr) 2017-12-21 2017-12-21 Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication

Publications (2)

Publication Number Publication Date
EP3502785A1 EP3502785A1 (fr) 2019-06-26
EP3502785B1 true EP3502785B1 (fr) 2020-08-12

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EP17209682.8A Active EP3502785B1 (fr) 2017-12-21 2017-12-21 Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication

Country Status (5)

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US (2) US11586146B2 (zh)
EP (1) EP3502785B1 (zh)
JP (3) JP6764915B2 (zh)
CN (1) CN109946945B (zh)
RU (1) RU2696327C1 (zh)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3502288B1 (fr) 2017-12-21 2020-10-14 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie
EP3422116B1 (fr) 2017-06-26 2020-11-04 Nivarox-FAR S.A. Ressort spiral d'horlogerie
EP3422115B1 (fr) 2017-06-26 2021-08-04 Nivarox-FAR S.A. Ressort spiralé d'horlogerie

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP3502289B1 (fr) * 2017-12-21 2022-11-09 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie
EP3796101A1 (fr) * 2019-09-20 2021-03-24 Nivarox-FAR S.A. Ressort spiral pour mouvement d'horlogerie
EP3828642A1 (fr) * 2019-11-29 2021-06-02 Nivarox-FAR S.A. Ressort spiral pour mouvement d'horlogerie et son procédé de fabrication
EP4009114A1 (fr) * 2019-12-31 2022-06-08 Nivarox-FAR S.A. Ressort spiral pour mouvement d'horlogerie et son procede de fabrication
EP4019459A1 (fr) * 2020-12-24 2022-06-29 Atokalpa, succursale de Alle de SFF Composants Horlogers S.A. Procédé de fabrication d'un ressort spiral thermocompensé
EP4060425A1 (fr) * 2021-03-16 2022-09-21 Nivarox-FAR S.A. Spiral pour un mouvement horloger
EP4060424A1 (fr) * 2021-03-16 2022-09-21 Nivarox-FAR S.A. Spiral pour mouvement d'horlogerie

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WO2015189278A2 (fr) 2014-06-11 2015-12-17 Cartier Création Studio Sa Oscillateur pour un ensemble de balancier-spiral d'une pièce d'horlogerie
EP2993531A1 (de) * 2014-09-08 2016-03-09 Precision Engineering AG Verfahren zur umformung einer feder
EP3002638A2 (fr) 2014-09-08 2016-04-06 Richemont International S.A. Procédé de fabrication d'un ressort spiral thermocompensé
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EP3422115A1 (fr) 2017-06-26 2019-01-02 Nivarox-FAR S.A. Ressort spiralé d'horlogerie
EP3422116B1 (fr) 2017-06-26 2020-11-04 Nivarox-FAR S.A. Ressort spiral d'horlogerie

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Cited By (3)

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Publication number Priority date Publication date Assignee Title
EP3422116B1 (fr) 2017-06-26 2020-11-04 Nivarox-FAR S.A. Ressort spiral d'horlogerie
EP3422115B1 (fr) 2017-06-26 2021-08-04 Nivarox-FAR S.A. Ressort spiralé d'horlogerie
EP3502288B1 (fr) 2017-12-21 2020-10-14 Nivarox-FAR S.A. Procédé de fabrication d'un ressort spiral pour mouvement d'horlogerie

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US20190196405A1 (en) 2019-06-27
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CN109946945B (zh) 2021-04-20
JP2020187134A (ja) 2020-11-19
JP6764915B2 (ja) 2020-10-07
CN109946945A (zh) 2019-06-28
JP2019113528A (ja) 2019-07-11
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US11586146B2 (en) 2023-02-21
US20230088320A1 (en) 2023-03-23

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