EP4214581A1 - Method for manufacturing a micromechanical component, in particular a timepiece mobile having an optimised surface - Google Patents

Method for manufacturing a micromechanical component, in particular a timepiece mobile having an optimised surface

Info

Publication number
EP4214581A1
EP4214581A1 EP21769741.6A EP21769741A EP4214581A1 EP 4214581 A1 EP4214581 A1 EP 4214581A1 EP 21769741 A EP21769741 A EP 21769741A EP 4214581 A1 EP4214581 A1 EP 4214581A1
Authority
EP
European Patent Office
Prior art keywords
mobile
phosphorus
substrate
chosen
nickel
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.)
Pending
Application number
EP21769741.6A
Other languages
German (de)
French (fr)
Inventor
Serge Nicoud
Samuel VIGNIER
Sébastien RODER
Jean-Luc Helfer
Christian Charbon
Frédéric Kohler
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.)
ETA SA Manufacture Horlogere Suisse
Original Assignee
ETA SA Manufacture Horlogere Suisse
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 ETA SA Manufacture Horlogere Suisse filed Critical ETA SA Manufacture Horlogere Suisse
Publication of EP4214581A1 publication Critical patent/EP4214581A1/en
Pending legal-status Critical Current

Links

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
    • G04B15/00—Escapements
    • G04B15/14—Component parts or constructional details, e.g. construction of the lever or the escape wheel
    • 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
    • G04B31/00—Bearings; Point suspensions or counter-point suspensions; Pivot bearings; Single parts therefor
    • G04B31/08—Lubrication

Definitions

  • the invention relates to a method for manufacturing a micromechanical component, in particular a horological mobile.
  • the invention relates to the field of horological mechanisms, and more particularly to escapement mechanisms comprising at least one escape wheel and at least one anchor, at least one of which is non-magnetic in nature.
  • the Swiss lever escapement wheels are historically made of nickel-plated steel, and are sensitive to magnetic fields.
  • the invention proposes to solve the technical problem of the behavior of the usual watch lubricant, and more particularly to guarantee an epilame effect, under the usual climatic conditions, on components in LIGA NiP12, or similar, non-ferromagnetic, especially on levers and Swiss lever escapement wheels.
  • the invention relates to a method of manufacturing watch mobiles according to claim 1.
  • the invention relates to the field of micromechanical components, and more particularly to horological mobiles.
  • the invention proposes to solve in particular the technical problem of the behavior of the usual watchmaking lubricant, in the usual climatic conditions, on components made of LIGA NiP12, or similar, non-ferromagnetic, in particular on the wheels of an escapement mechanism. Swiss anchor.
  • the contact between the ruby lever of the anchor and the tooth of the escapement wheel is particularly sensitive, as is the contact between the fork and the plate peg. or between the fork and the anchor stops.
  • this involves ensuring the presence of lubricant on the contact surfaces between the escape wheel and the pallet, and reducing the aging of the escape wheel and the pallet.
  • the main problem is the loss of epilame effect on the escape wheel plate, which causes oil spreading and loss of lubrication at the contact between the wheel tooth and the ruby lift.
  • the stability of the lubrication in contact between the lifts of the anchor and the escapement wheel must make it possible to guarantee the constancy of the amplitude.
  • a coating in the form of a layer of galvanic nickel (Ni) preferentially, or of chemical nickel (for example NiP6-9), or else of nickel-boron deposited by chemical means, on a LIGA NiP12 escape wheel greatly improves movement performance.
  • the galvanic nickel coating may be an alloy, for example Ni-Fe, or Ni-W, or other.
  • the invention relates to a process for manufacturing a micromechanical component, in particular a watch mobile, according to which a substrate is produced with a first material comprising at least nickel and phosphorus, this substrate is shaped by geometry of the mobile, and the substrate is coated, by galvanic and/or chemical means, at the level of at least one surface of the substrate of the mobile, with at least a second thin material, less than 10 micrometers, which constitutes a peripheral layer of the mobile at the level of this at least one surface of the substrate of the mobile, and which comprises at least nickel and which is poorer in phosphorus than the first material, or which comprises nickel and is devoid of phosphorus.
  • this first non-magnetic material is chosen.
  • this second non-magnetic material is chosen. More precisely, it has an amagnetic character.
  • nickel is not non-magnetic, and that NiP6-9% is not necessarily so, it is the low thickness of the deposit which gives the part its non-magnetic character.
  • the substrate is a nickel-phosphorus of NiPx formulation, with x comprised between 1% and 15% by mass, or more particularly with x comprised between 10% and 15% by mass, this latter range making it possible to guarantee the non-magnetic nature of the coating.
  • the coating covering the substrate is low in phosphorus, and its thickness is not limited to between 0.2 micrometers and 10.0 micrometers, and more particularly still between 0.2 micrometers and 2.0 micrometers.
  • the coating has a thickness of 0.5 micrometer.
  • the coating treatment with a coating low in phosphorus, according to the invention, can be carried out by galvanic means.
  • the coating treatment with a low or zero phosphorus coating can be done chemically, according to a method of applying chemical nickel, which can be pure nickel, or else a nickel- phosphorus low in phosphorus, for example NiP6-9, with 6% to 9% by mass of phosphorus, or even a nickel-boron NiB.
  • chemical nickel which can be pure nickel, or else a nickel- phosphorus low in phosphorus, for example NiP6-9, with 6% to 9% by mass of phosphorus, or even a nickel-boron NiB.
  • the epilame used is a fluorine-based formulation.
  • the lubricant can also be deposited on an escapement wheel set with a supplement in the form of a paste based on molybdenum disulphide MoS2, which acts as a lubricant and a lubricant sponge.
  • the escapement wheel concerned has a geometry making it possible to reduce the contact surfaces to a minimum, for example the use of a cradled anchor is preferred, which is an anchor whose active faces of the fork, intended to come into contact with the chainring pin and the stops, are rounded, which makes it possible to have a point of contact instead of a line of contact.
  • a cradled anchor is preferred, which is an anchor whose active faces of the fork, intended to come into contact with the chainring pin and the stops, are rounded, which makes it possible to have a point of contact instead of a line of contact.
  • An innovative embodiment of an escapement mechanism comprises an anchor in LIGA, or an anchor whose pallets at least are in LIGA.
  • the LIGA parts of the anchor are subject to the same problem, and the same solution is applicable.
  • the invention makes it possible to guarantee normal aging conditions, constant amplitude, and the absence of shutdown, in particular in the presence of cradled LIGA nickel-phosphorus anchors, which provide better shock resistance than anchors silicon, for example.
  • a process for manufacturing a clockwork mobile is implemented, according to which:
  • a substrate is manufactured with a first material comprising at least nickel and phosphorus
  • This substrate is coated, at at least one surface of the mobile substrate, with at least one second material which constitutes a peripheral layer of the mobile at this at least one surface of the substrate;
  • This at least one second material comprises at least nickel, and is poorer in phosphorus than the first material, or else this at least one second material comprises nickel and is devoid of phosphorus.
  • this coating of the substrate is carried out, at the level of at least one surface adjoining a friction surface of the mobile, with this at least one second material, which constitutes a peripheral layer of the mobile at the level of this at least one surface adjoining a rubbing surface.
  • “adjoining” we mean that the two surfaces are contiguous, or at least tangent, their intersection is not empty, even if it is limited to an isthmus of very small section.
  • the substrate is shaped to the geometry of the mobile.
  • this coating of the substrate is carried out by galvanic and/or chemical and/or PVD and/or CVD means.
  • this coating of the substrate is carried out at surfaces of the mobile other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom. More particularly, this coating of the substrate is carried out at all the surfaces of the mobile other than these guide surfaces of the mobile.
  • the coating of the substrate is carried out at the surfaces of the mobile including these guide surfaces of the mobile. In yet another variant, this coating is carried out at the level of at least one surface adjoining a friction surface of the mobile, other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom. More particularly, this coating of the substrate is carried out at all the surfaces of the mobile other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom.
  • the coating of the substrate is carried out at the level of surfaces adjoining a friction surface of the mobile including the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom.
  • the coating of the substrate is carried out at all the surfaces of the mobile.
  • the first material comprising phosphorus with a mass proportion of between 1% and 15% is chosen.
  • the first material consisting solely of nickel and phosphorus is chosen.
  • the first non-magnetic material is chosen with a mass proportion of phosphorus of between 10% and 15%.
  • the first non-magnetic material is chosen.
  • the second material is chosen comprising only pure nickel, or else only nickel and phosphorus.
  • the second material is chosen with a phosphorus mass proportion of less than or equal to 15%.
  • the second non-magnetic material is chosen with a mass proportion of phosphorus of between 10% and 15%.
  • the second material is chosen with a mass proportion of phosphorus of between 6% and 12%.
  • the second material is chosen with a mass proportion of phosphorus of between 1% and 6%. In yet another alternative, the second material is chosen with a mass proportion of phosphorus less than or equal to 1%.
  • the second material comprising boron is chosen.
  • the second material consisting solely of nickel and boron is chosen.
  • the second material is applied galvanically.
  • the second material is applied chemically.
  • the coating is applied with a thickness of less than 10 micrometers.
  • the coating is applied with a thickness of between 0.2 micrometer and 5.0 micrometer. More particularly still, the coating is applied with a thickness of between 0.2 micrometer and 2.0 micrometer.
  • the coating is applied with a thickness of less than 0.2 micrometer, in particular in the vicinity of 0.1 micrometer.
  • a heat treatment is applied to the assembly formed by the substrate and its coating, at a temperature of between 100° C. and 500° C., for 1 to 8 hours.
  • this heat treatment is carried out after the coating operation.
  • this heat treatment is carried out before the coating operation.
  • the substrate is produced by a “LIGA” process (lithography-galvanization-forming, from the German “Rôntgenlithographie, Galvanoformung, Abformung”).
  • a coating is carried out by galvanic and/or chemical means of all the surfaces of the substrate, with such a second material.
  • this process is applied to the manufacture of an escape wheel set formed for example by an escape wheel or an anchor.
  • the thickness of the second material which constitutes the peripheral layer of the mobile is limited at the level of the at least one surface adjoining a friction surface to less than 10 micrometers. Even more particularly, the thickness of the second material which constitutes the peripheral layer of the mobile at the level of the at least one surface adjoining a friction surface is limited to less than 5 micrometers.
  • the thickness of the second material which constitutes the peripheral layer of the mobile at the level of at least one surface of the substrate is limited to less than 10 micrometers. Even more particularly, the thickness of the second material which constitutes the peripheral layer of the mobile at the level of the at least one surface of the substrate is limited to less than 5 micrometers.
  • This process allows the production of a micromechanical component, in particular a horological mobile, and more particularly still an escapement mechanism mobile, the surface of which is optimized.
  • the mobile thus manufactured can advantageously receive, on its friction surfaces, a lubricating substance, for example a synthetic oil or grease suitable for precision microtechnology applications, known to those skilled in the watchmaking profession.
  • a lubricating substance for example a synthetic oil or grease suitable for precision microtechnology applications, known to those skilled in the watchmaking profession.
  • Such a lubricating substance can be combined with a paste based on molybdenum disulphide MoS2.
  • the mobile can advantageously also receive a layer of epilame on at least one surface of the coating other than its friction surfaces in order to allow a better hold of the lubricating substance.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Micromachines (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)
  • Chemically Coating (AREA)
  • Lubricants (AREA)

Abstract

Method for manufacturing a timepiece mobile, in which a substrate is produced with a first material comprising at least nickel and phosphorus, the substrate is shaped to the geometry of the mobile, and the substrate is galvanically or chemically coated, on at least one surface of the mobile substrate, with at least one second material which constitutes the peripheral layer of the mobile on the at least one surface of the mobile substrate, and which comprises at least nickel and which has less phosphorus than the first material, or which comprises nickel and lacks phosphorus.

Description

PROCEDE DE FABRICATION D’UN COMPOSANT DE MICROMECANIQUE, NOTAMMENT D’UN MOBILE D’HORLOGERIE, DONT LA SURFACE EST OPTIMISEE METHOD FOR MANUFACTURING A MICROMECHANICAL COMPONENT, IN PARTICULAR A CLOCK MOBILE, WHOSE SURFACE IS OPTIMIZED
Domaine de l’invention Field of invention
L’invention concerne un procédé de fabrication d’un composant de micromécanique, notamment d’un mobile d’horlogerie. The invention relates to a method for manufacturing a micromechanical component, in particular a horological mobile.
L’invention concerne le domaine des mécanismes d’horlogerie, et plus particulièrement des mécanismes d’échappement comportant au moins une roue d’échappement et au moins une ancre, dont au moins l’un d’eux est à caractère amagnétique. The invention relates to the field of horological mechanisms, and more particularly to escapement mechanisms comprising at least one escape wheel and at least one anchor, at least one of which is non-magnetic in nature.
Arrière-plan de l’invention Background of the invention
Dans les mécanismes d’échappement d’horlogerie à ancre suisse, les roues d’échappement à ancre suisse sont historiquement en acier nickelé, et sont sensibles aux champs magnétiques. In Swiss lever timepiece escapement mechanisms, the Swiss lever escapement wheels are historically made of nickel-plated steel, and are sensitive to magnetic fields.
On connaît des alternatives avec des matériaux comme le nickel-phosphore Ni P 12 mis en œuvre par procédé « LIGA » (Lithographie und Galvano-Abformung », qui ont un comportement amagnétique. Alternatives are known with materials such as nickel-phosphorus Ni P 12 implemented by the “LIGA” (Lithographie und Galvano-Abformung) process, which have a non-magnetic behavior.
Toutefois l’emploi de tels matériaux, nickel-phosphore, ou analogues, peut se révéler sensible dans certaines conditions climatiques, qui sont susceptibles d’entraîner une dégradation des performances, notamment en termes de régularité d’amplitude, d’arrêts, ou encore de vieillissement, surtout quand les deux composants antagonistes du couple de frottement sont réalisés dans des matériaux LIGA similaires. However, the use of such materials, nickel-phosphorus, or the like, may prove to be sensitive under certain climatic conditions, which are likely to lead to a deterioration in performance, in particular in terms of amplitude regularity, stops, or even aging, especially when the two opposing components of the friction couple are made of similar LIGA materials.
Résumé de l’invention Summary of the invention
L’invention se propose de résoudre le problème technique de la tenue du lubrifiant horloger habituel, et plus particulièrement de garantir un effet épilame, dans les conditions climatiques usuelles, sur des composants en LIGA NiP12, ou similaire, non ferromagnétique, en particulier sur des ancres et des roues d’échappement à ancre suisse. The invention proposes to solve the technical problem of the behavior of the usual watch lubricant, and more particularly to guarantee an epilame effect, under the usual climatic conditions, on components in LIGA NiP12, or similar, non-ferromagnetic, especially on levers and Swiss lever escapement wheels.
A cet effet, l’invention concerne un procédé de fabrication de mobiles d’horlogerie selon la revendication 1. To this end, the invention relates to a method of manufacturing watch mobiles according to claim 1.
Description détaillée des modes de réalisation préférés Detailed Description of Preferred Embodiments
L’invention concerne le domaine des composants de micromécanique, et plus particulièrement des mobiles d’horlogerie. The invention relates to the field of micromechanical components, and more particularly to horological mobiles.
L’invention se propose de résoudre notamment le problème technique de la tenue du lubrifiant horloger habituel, dans les conditions climatiques usuelles, sur des composants en LIGA NiP12, ou similaire, non ferromagnétique, en particulier sur des roues d’un mécanisme d’échappement à ancre suisse. The invention proposes to solve in particular the technical problem of the behavior of the usual watchmaking lubricant, in the usual climatic conditions, on components made of LIGA NiP12, or similar, non-ferromagnetic, in particular on the wheels of an escapement mechanism. Swiss anchor.
Dans les mécanismes d’échappement d’horlogerie à ancre suisse, le contact entre la levée en rubis de l’ancre et la dent de la roue d’échappement est particulièrement sensible, de même que le contact entre la fourchette et la cheville de plateau ou entre la fourchette et les butées d’ancre. In Swiss lever watchmaking escapement mechanisms, the contact between the ruby lever of the anchor and the tooth of the escapement wheel is particularly sensitive, as is the contact between the fork and the plate peg. or between the fork and the anchor stops.
Il s’agit en particulier d’assurer la présence de lubrifiant sur les surfaces de contact entre la roue d’échappement et l’ancre, et de réduire le vieillissement de la roue d’échappement et de l’ancre. In particular, this involves ensuring the presence of lubricant on the contact surfaces between the escape wheel and the pallet, and reducing the aging of the escape wheel and the pallet.
Le problème principal est la perte d’effet épilame sur la planche de la roue d’échappement, qui provoque un étalement de l’huile et une perte de lubrification au contact entre la dent de la roue et la levée en rubis. The main problem is the loss of epilame effect on the escape wheel plate, which causes oil spreading and loss of lubrication at the contact between the wheel tooth and the ruby lift.
La stabilité de la lubrification au contact entre les levées de l’ancre et la roue d’échappement doit permettre de garantir la constance de l’amplitude. The stability of the lubrication in contact between the lifts of the anchor and the escapement wheel must make it possible to guarantee the constancy of the amplitude.
A cet effet, l’ajout d’un revêtement sous la forme d’une couche de nickel galvanique (Ni) préférentiellement, ou de nickel chimique (par exemple NiP6-9), ou encore de nickel-bore déposé par voie chimique, sur une roue d’échappement en LIGA NiP12 permet d’améliorer grandement les performances des mouvements. For this purpose, the addition of a coating in the form of a layer of galvanic nickel (Ni) preferentially, or of chemical nickel (for example NiP6-9), or else of nickel-boron deposited by chemical means, on a LIGA NiP12 escape wheel greatly improves movement performance.
En effet, il a été démontré par différents tests que cette amélioration notable est liée à une meilleure tenue de l’épilame en conditions climatiques prédéterminées, par exemple à 50° Celsius et à un taux d’hygrométrie de 90%. Un meilleur accrochage de l’épilame sur la matière a été constaté par les inventeurs, quand la quantité de phosphore en surface est réduite, et par conséquent, la tenue du lubrifiant est d’autant meilleure que la quantité de phosphore est faible. Indeed, it has been demonstrated by various tests that this significant improvement is linked to a better hold of the epilame in climatic conditions. predetermined, for example at 50° Celsius and at a humidity level of 90%. Better attachment of the epilame to the material has been observed by the inventors, when the quantity of surface phosphorus is reduced, and consequently, the behavior of the lubricant is all the better as the quantity of phosphorus is low.
Dans une variante, le revêtement de nickel galvanique peut être un alliage, par exemple Ni-Fe, ou Ni-W, ou autre. Alternatively, the galvanic nickel coating may be an alloy, for example Ni-Fe, or Ni-W, or other.
Ainsi l’invention concerne un procédé de fabrication de composant de micromécanique, notamment d’un mobile d’horlogerie, selon lequel on réalise un substrat avec un premier matériau comportant au moins du nickel et du phosphore, on met en forme ce substrat à la géométrie du mobile, et on effectue un revêtement du substrat, par voie galvanique et/ou chimique, au niveau d’au moins une surface du substrat du mobile, avec au moins un deuxième matériau de faible épaisseur, inférieure à 10 micromètres, qui constitue une couche périphérique du mobile au niveau de cette au moins une surface du substrat du mobile, et qui comporte au moins du nickel et qui est plus pauvre en phosphore que le premier matériau, ou qui comporte du nickel et est dépourvu de phosphore. Thus the invention relates to a process for manufacturing a micromechanical component, in particular a watch mobile, according to which a substrate is produced with a first material comprising at least nickel and phosphorus, this substrate is shaped by geometry of the mobile, and the substrate is coated, by galvanic and/or chemical means, at the level of at least one surface of the substrate of the mobile, with at least a second thin material, less than 10 micrometers, which constitutes a peripheral layer of the mobile at the level of this at least one surface of the substrate of the mobile, and which comprises at least nickel and which is poorer in phosphorus than the first material, or which comprises nickel and is devoid of phosphorus.
Plus particulièrement, on choisit ce premier matériau amagnétique. More particularly, this first non-magnetic material is chosen.
Plus particulièrement, on choisit ce deuxième matériau amagnétique. Plus précisément, il présente un caractère amagnétique. More particularly, this second non-magnetic material is chosen. More precisely, it has an amagnetic character.
On remarque que le nickel n’est pas amagnétique, et que le NiP6-9% ne l’est pas forcément, c’est la faible épaisseur du dépôt qui confère à la pièce son caractère amagnétique Note that nickel is not non-magnetic, and that NiP6-9% is not necessarily so, it is the low thickness of the deposit which gives the part its non-magnetic character.
Dans une réalisation particulière, le substrat est un nickel-phosphore de formulation NiPx, avec x compris entre 1 % et 15% en masse, ou plus particulièrement avec x compris entre 10% et 15% en masse, cette dernière plage permettant de garantir le caractère amagnétique du revêtement. In a particular embodiment, the substrate is a nickel-phosphorus of NiPx formulation, with x comprised between 1% and 15% by mass, or more particularly with x comprised between 10% and 15% by mass, this latter range making it possible to guarantee the non-magnetic nature of the coating.
Le revêtement recouvrant le substrat est pauvre en phosphore, et son épaisseur est non limitativement comprise entre 0.2 micromètre et 10.0 micromètres, et, plus particulièrement encore comprise entre 0.2 micromètre et 2.0 micromètres. The coating covering the substrate is low in phosphorus, and its thickness is not limited to between 0.2 micrometers and 10.0 micrometers, and more particularly still between 0.2 micrometers and 2.0 micrometers.
Préférentiellement, le revêtement présente une épaisseur de 0,5 micromètre. Le traitement de recouvrement avec un revêtement pauvre en phosphore, selon l’invention, peut se faire par voie galvanique. Preferably, the coating has a thickness of 0.5 micrometer. The coating treatment with a coating low in phosphorus, according to the invention, can be carried out by galvanic means.
Il est possible d’appliquer un traitement thermique au substrat avant l’opération de dépôt, notamment galvanique, ou bien, encore, d’appliquer un traitement thermique à l’ensemble formé par le substrat et son revêtement après l’opération de dépôt, notamment galvanique. It is possible to apply a heat treatment to the substrate before the deposition operation, in particular galvanic, or even to apply a heat treatment to the assembly formed by the substrate and its coating after the deposition operation, particularly galvanic.
Il est aussi possible d’appliquer un traitement chimique au substrat pour modifier ses caractéristiques superficielles de façon à faciliter l’accroche du revêtement, notamment par voie galvanique. It is also possible to apply a chemical treatment to the substrate to modify its surface characteristics so as to facilitate the adhesion of the coating, in particular by galvanic means.
En alternative, le traitement de recouvrement avec un revêtement pauvre ou nul en phosphore, selon l’invention, peut se faire par voie chimique, selon un procédé d’application de nickel chimique, qui peut être du nickel pur, ou bien un nickel-phosphore pauvre en phosphore, par exemple de NiP6-9, avec de 6% à 9% en masse de phosphore, ou bien encore un nickel-bore NiB. Alternatively, the coating treatment with a low or zero phosphorus coating, according to the invention, can be done chemically, according to a method of applying chemical nickel, which can be pure nickel, or else a nickel- phosphorus low in phosphorus, for example NiP6-9, with 6% to 9% by mass of phosphorus, or even a nickel-boron NiB.
L’ajout d’une couche de nickel, ou de NiP6-9, ou de NiB, permet d’augmenter la stabilité de l’épilame en toutes conditions climatiques, l’accroche de l’épilame et donc la tenue de n’importe quel lubrifiant horloger usuel. The addition of a layer of nickel, or of NiP6-9, or of NiB, makes it possible to increase the stability of the epilame in all climatic conditions, the grip of the epilame and therefore the holding of any what usual watch lubricant.
Plus particulièrement, l’épilame utilisé est une formulation à base de fluor.More particularly, the epilame used is a fluorine-based formulation.
Le lubrifiant peut, encore, être déposé sur un mobile d’échappement avec un complément sous forme d’une pâte à base de bisulfure de molybdène MoS2, qui joue le rôle de lubrifiant et d’éponge à lubrifiant. The lubricant can also be deposited on an escapement wheel set with a supplement in the form of a paste based on molybdenum disulphide MoS2, which acts as a lubricant and a lubricant sponge.
De façon avantageuse, le mobile d’échappement concerné a une géométrie permettant de réduire au minimum les surfaces de contact, par exemple on privilégie l’emploi d’une ancre bercée, qui est une ancre dont les faces actives de la fourchette, destinées à venir en contact avec la cheville de plateau et les butées, sont arrondies, ce qui permet d’avoir un point de contact à la place d’une ligne de contact. Advantageously, the escapement wheel concerned has a geometry making it possible to reduce the contact surfaces to a minimum, for example the use of a cradled anchor is preferred, which is an anchor whose active faces of the fork, intended to come into contact with the chainring pin and the stops, are rounded, which makes it possible to have a point of contact instead of a line of contact.
Une réalisation innovante de mécanisme d’échappement comporte une ancre en LIGA, ou une ancre dont au moins les palettes sont en LIGA. Dans un tel cas, les parties en LIGA de l’ancre sont soumises au même problème, et la même solution est applicable. L’invention permet de garantir des conditions de vieillissement normal, une constance de l’amplitude, et l’absence d’arrêt, notamment en présence d’ancres en nickel-phosphore LIGA bercées, lesquelles assurent une meilleure tenue au choc que des ancres en silicium, par exemple. An innovative embodiment of an escapement mechanism comprises an anchor in LIGA, or an anchor whose pallets at least are in LIGA. In such a case, the LIGA parts of the anchor are subject to the same problem, and the same solution is applicable. The invention makes it possible to guarantee normal aging conditions, constant amplitude, and the absence of shutdown, in particular in the presence of cradled LIGA nickel-phosphorus anchors, which provide better shock resistance than anchors silicon, for example.
Ainsi, de façon préférée, on met en œuvre un procédé de fabrication d’un mobile d’horlogerie, selon lequel : Thus, preferably, a process for manufacturing a clockwork mobile is implemented, according to which:
- on fabrique un substrat avec un premier matériau comportant au moins du nickel et du phosphore, et - a substrate is manufactured with a first material comprising at least nickel and phosphorus, and
- on effectue un revêtement de ce substrat, au niveau d’au moins une surface du substrat du mobile, avec au moins un deuxième matériau qui constitue une couche périphérique du mobile au niveau de cette au moins une surface du substrat ; - This substrate is coated, at at least one surface of the mobile substrate, with at least one second material which constitutes a peripheral layer of the mobile at this at least one surface of the substrate;
- cet au moins un deuxième matériau comporte au moins du nickel, et est plus pauvre en phosphore que le premier matériau, ou bien cet au moins un deuxième matériau comporte du nickel et est dépourvu de phosphore. - This at least one second material comprises at least nickel, and is poorer in phosphorus than the first material, or else this at least one second material comprises nickel and is devoid of phosphorus.
Plus particulièrement, on effectue ce revêtement du substrat, au niveau d’au moins une surface jouxtant une surface frottante du mobile, avec cet au moins un deuxième matériau, qui constitue une couche périphérique du mobile au niveau de cette au moins une surface jouxtant une surface frottante. Par « jouxtant » on entend que les deux surfaces sont contiguës, ou au moins tangentes, leur intersection n’est pas vide, même si elle est limitée à un isthme de très petite section. More particularly, this coating of the substrate is carried out, at the level of at least one surface adjoining a friction surface of the mobile, with this at least one second material, which constitutes a peripheral layer of the mobile at the level of this at least one surface adjoining a rubbing surface. By "adjoining" we mean that the two surfaces are contiguous, or at least tangent, their intersection is not empty, even if it is limited to an isthmus of very small section.
Plus particulièrement, on met en forme le substrat à la géométrie du mobile.More particularly, the substrate is shaped to the geometry of the mobile.
Plus particulièrement, on effectue ce revêtement du substrat par voie galvanique et/ou chimique et/ou PVD et/ou CVD. More particularly, this coating of the substrate is carried out by galvanic and/or chemical and/or PVD and/or CVD means.
Dans une variante, on effectue ce revêtement du substrat au niveau de surfaces du mobile autres que les surfaces de guidage du mobile pour son pivotement ou pour son guidage selon un degré de liberté unique. Plus particulièrement, on effectue ce revêtement du substrat au niveau de toutes les surfaces du mobile autres que ces surfaces de guidage du mobile. In a variant, this coating of the substrate is carried out at surfaces of the mobile other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom. More particularly, this coating of the substrate is carried out at all the surfaces of the mobile other than these guide surfaces of the mobile.
Dans une autre variante, on effectue le revêtement du substrat au niveau de surfaces du mobile y compris ces surfaces de guidage du mobile. Dans une autre variante encore, on effectue ce revêtement au niveau d’au moins une surface jouxtant une surface frottante du mobile, autres que les surfaces de guidage du mobile pour son pivotement ou pour son guidage selon un degré de liberté unique. Plus particulièrement, on effectue ce revêtement du substrat au niveau de toutes les surfaces du mobile autres que les surfaces de guidage du mobile pour son pivotement ou pour son guidage selon un degré de liberté unique. In another variant, the coating of the substrate is carried out at the surfaces of the mobile including these guide surfaces of the mobile. In yet another variant, this coating is carried out at the level of at least one surface adjoining a friction surface of the mobile, other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom. More particularly, this coating of the substrate is carried out at all the surfaces of the mobile other than the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom.
Dans encore une autre variante, on effectue le revêtement du substrat au niveau de surfaces jouxtant une surface frottante du mobile y compris les surfaces de guidage du mobile pour son pivotement ou pour son guidage selon un degré de liberté unique. In yet another variant, the coating of the substrate is carried out at the level of surfaces adjoining a friction surface of the mobile including the guide surfaces of the mobile for its pivoting or for its guidance according to a single degree of freedom.
Dans une variante, on effectue le revêtement du substrat au niveau de toutes les surfaces du mobile. In a variant, the coating of the substrate is carried out at all the surfaces of the mobile.
Plus particulièrement, on choisit le premier matériau comportant du phosphore avec une proportion en masse comprise entre 1% et 15%. More particularly, the first material comprising phosphorus with a mass proportion of between 1% and 15% is chosen.
Plus particulièrement, on choisit le premier matériau constitué uniquement de nickel et de phosphore. More particularly, the first material consisting solely of nickel and phosphorus is chosen.
Plus particulièrement, on choisit le premier matériau amagnétique avec une proportion en masse de phosphore comprise entre 10% et 15%. More particularly, the first non-magnetic material is chosen with a mass proportion of phosphorus of between 10% and 15%.
Plus particulièrement, on choisit le premier matériau amagnétique. More particularly, the first non-magnetic material is chosen.
Plus particulièrement, on choisit le deuxième matériau comportant uniquement du nickel pur, ou bien uniquement du nickel et du phosphore. More particularly, the second material is chosen comprising only pure nickel, or else only nickel and phosphorus.
Plus particulièrement, on choisit le deuxième matériau avec une proportion en masse de phosphore inférieure ou égale à 15%. More particularly, the second material is chosen with a phosphorus mass proportion of less than or equal to 15%.
Plus particulièrement, on choisit le deuxième matériau amagnétique avec une proportion en masse de phosphore comprise entre 10% et 15%. More particularly, the second non-magnetic material is chosen with a mass proportion of phosphorus of between 10% and 15%.
Dans une alternative, on choisit le deuxième matériau avec une proportion en masse de phosphore comprise entre 6% et 12%. Alternatively, the second material is chosen with a mass proportion of phosphorus of between 6% and 12%.
Dans une autre alternative, on choisit le deuxième matériau avec une proportion en masse de phosphore comprise entre 1 % et 6%. Dans une autre alternative encore, on choisit le deuxième matériau avec une proportion en masse de phosphore inférieure ou égale à 1%. In another alternative, the second material is chosen with a mass proportion of phosphorus of between 1% and 6%. In yet another alternative, the second material is chosen with a mass proportion of phosphorus less than or equal to 1%.
Plus particulièrement, on choisit le deuxième matériau comportant du bore.More particularly, the second material comprising boron is chosen.
Plus particulièrement encore, on choisit le deuxième matériau constitué uniquement de nickel et de bore. Even more particularly, the second material consisting solely of nickel and boron is chosen.
Dans une variante, on applique le deuxième matériau par voie galvanique.In a variant, the second material is applied galvanically.
Dans une autre variante, on applique le deuxième matériau par voie chimique. In another variant, the second material is applied chemically.
Plus particulièrement, on applique le revêtement avec une épaisseur inférieure à 10 micromètres. More particularly, the coating is applied with a thickness of less than 10 micrometers.
Plus particulièrement, on applique le revêtement avec une épaisseur comprise entre 0.2 micromètre et 5.0 micromètre. Plus particulièrement encore, on applique le revêtement avec une épaisseur comprise entre 0.2 micromètre et 2.0 micromètre. More particularly, the coating is applied with a thickness of between 0.2 micrometer and 5.0 micrometer. More particularly still, the coating is applied with a thickness of between 0.2 micrometer and 2.0 micrometer.
Dans une autre variante encore, on applique le revêtement avec une épaisseur inférieure à 0.2 micromètre, notamment au voisinage de 0.1 micromètre. In yet another variant, the coating is applied with a thickness of less than 0.2 micrometer, in particular in the vicinity of 0.1 micrometer.
Plus particulièrement, on applique un traitement thermique à l’ensemble formé par le substrat et son revêtement, à une température comprise entre 100°C et 500°C, pendant 1 à 8 heures. Dans une alternative, on effectue ce traitement thermique après l’opération de revêtement. Dans une autre alternative, on effectue ce traitement thermique avant l’opération de revêtement. More particularly, a heat treatment is applied to the assembly formed by the substrate and its coating, at a temperature of between 100° C. and 500° C., for 1 to 8 hours. Alternatively, this heat treatment is carried out after the coating operation. In another alternative, this heat treatment is carried out before the coating operation.
Plus particulièrement, on réalise le substrat par un procédé « LIGA » (lithographie-galvanisation-formage, de l’allemand « Rôntgenlithographie, Galvanoformung, Abformung). More particularly, the substrate is produced by a “LIGA” process (lithography-galvanization-forming, from the German “Rôntgenlithographie, Galvanoformung, Abformung”).
Plus particulièrement, on effectue un revêtement par voie galvanique et/ou chimique de toutes les surfaces du substrat, avec un tel deuxième matériau. More particularly, a coating is carried out by galvanic and/or chemical means of all the surfaces of the substrate, with such a second material.
Plus particulièrement, on applique ce procédé à la fabrication d’un mobile d’échappement formé par exemple par une roue d’échappement ou une ancre. More particularly, this process is applied to the manufacture of an escape wheel set formed for example by an escape wheel or an anchor.
Dans une variante, on limite l’épaisseur du deuxième matériau qui constitue la couche périphérique du mobile au niveau de la au moins une surface jouxtant une surface frottante à moins de 10 micromètres. Plus particulièrement encore, on limite l’épaisseur du deuxième matériau qui constitue la couche périphérique du mobile au niveau de la au moins une surface jouxtant une surface frottante à moins de 5 micromètres. In a variant, the thickness of the second material which constitutes the peripheral layer of the mobile is limited at the level of the at least one surface adjoining a friction surface to less than 10 micrometers. Even more particularly, the thickness of the second material which constitutes the peripheral layer of the mobile at the level of the at least one surface adjoining a friction surface is limited to less than 5 micrometers.
Dans une variante, on limite l’épaisseur du deuxième matériau qui constitue la couche périphérique du mobile au niveau de la au moins une surface du substrat à moins de 10 micromètres. Plus particulièrement encore, on limite l’épaisseur du deuxième matériau qui constitue la couche périphérique du mobile au niveau de la au moins une surface du substrat à moins de 5 micromètres. In a variant, the thickness of the second material which constitutes the peripheral layer of the mobile at the level of at least one surface of the substrate is limited to less than 10 micrometers. Even more particularly, the thickness of the second material which constitutes the peripheral layer of the mobile at the level of the at least one surface of the substrate is limited to less than 5 micrometers.
Ce procédé permet la réalisation d’un composant micromécanique, notamment un mobile d’horlogerie, et plus particulièrement encore un mobile de mécanisme d’échappement, dont la surface est optimisée. This process allows the production of a micromechanical component, in particular a horological mobile, and more particularly still an escapement mechanism mobile, the surface of which is optimized.
Le mobile ainsi fabriqué peut avantageusement recevoir, sur ses surfaces frottantes, une substance lubrifiante, par exemple une huile ou une graisse de synthèse adaptée aux applications microtechniques de précision, connue de l’homme du métier de l’horlogerie. Une telle substance lubrifiante peut être combinée à une pâte à base de bisulfure de molybdène MoS2. The mobile thus manufactured can advantageously receive, on its friction surfaces, a lubricating substance, for example a synthetic oil or grease suitable for precision microtechnology applications, known to those skilled in the watchmaking profession. Such a lubricating substance can be combined with a paste based on molybdenum disulphide MoS2.
Le mobile peut avantageusement également recevoir une couche d’épilame sur au moins une surface du revêtement autre que ses surfaces frottantes afin de permettre une meilleure tenue de la substance lubrifiante. The mobile can advantageously also receive a layer of epilame on at least one surface of the coating other than its friction surfaces in order to allow a better hold of the lubricating substance.

Claims

- 9 - REVEN DI CATI ONS - 9 - REVEN DI CATI ONS
1. Procédé de fabrication d’un mobile d’horlogerie, caractérisé en ce qu’on fabrique un substrat avec un premier matériau comportant au moins du nickel et du phosphore, et en ce qu’on effectue un revêtement dudit substrat, au niveau d’au moins une surface du substrat dudit mobile, avec au moins un deuxième matériau qui constitue une couche périphérique dudit mobile au niveau de ladite au moins une surface du substrat dudit mobile, et qui comporte au moins du nickel et qui est plus pauvre en phosphore que ledit premier matériau, ou qui comporte du nickel et est dépourvu de phosphore. 1. A method of manufacturing a watch mobile, characterized in that a substrate is manufactured with a first material comprising at least nickel and phosphorus, and in that said substrate is coated at the level of at least one surface of the substrate of said mobile, with at least one second material which constitutes a peripheral layer of said mobile at the level of said at least one surface of the substrate of said mobile, and which comprises at least nickel and which is poorer in phosphorus than said first material, or which comprises nickel and is devoid of phosphorus.
2. Procédé selon la revendication 1 , caractérisé en ce qu’on effectue ledit revêtement dudit substrat, au niveau d’au moins une surface jouxtant une surface frottante dudit mobile, avec ledit au moins un deuxième matériau qui constitue la couche périphérique dudit mobile au niveau de ladite au moins une surface jouxtant une surface frottante dudit mobile. 2. Method according to claim 1, characterized in that said coating of said substrate is carried out, at at least one surface adjoining a friction surface of said mobile, with said at least one second material which constitutes the peripheral layer of said mobile at the level of said at least one surface adjoining a friction surface of said mobile.
3. Procédé selon la revendication 1 ou 2, caractérisé en ce qu’on met en forme ledit substrat à la géométrie dudit mobile. 3. Method according to claim 1 or 2, characterized in that said substrate is shaped to the geometry of said mobile.
4. Procédé selon l’une des revendications 1 à 3, caractérisé en ce qu’on effectue ledit revêtement dudit substrat par voie galvanique et/ou chimique et/ou PVD et/ou CVD. 4. Method according to one of claims 1 to 3, characterized in that said coating of said substrate is carried out by galvanic and/or chemical and/or PVD and/or CVD means.
5. Procédé selon l’une des revendications 1 à 4, caractérisé en ce qu’on choisit ledit premier matériau constitué uniquement de nickel et de phosphore. 5. Method according to one of claims 1 to 4, characterized in that said first material is chosen consisting solely of nickel and phosphorus.
6. Procédé selon l’une des revendications 1 à 5, caractérisé en ce qu’on choisit ledit premier matériau avec une proportion en masse de phosphore comprise entre 1% et 15%. 6. Method according to one of claims 1 to 5, characterized in that said first material is chosen with a mass proportion of phosphorus between 1% and 15%.
7. Procédé selon l’une des revendications 1 à 6, caractérisé en ce qu’on choisit ledit premier matériau amagnétique avec une proportion en masse de phosphore comprise entre 10% et 15%. 7. Method according to one of claims 1 to 6, characterized in that said first non-magnetic material is chosen with a mass proportion of phosphorus of between 10% and 15%.
8. Procédé selon l’une des revendications 1 à 7, caractérisé en ce qu’on choisit ledit deuxième matériau comportant uniquement du nickel pur, ou bien uniquement du nickel et du phosphore. 8. Method according to one of claims 1 to 7, characterized in that said second material is chosen comprising only pure nickel, or else only nickel and phosphorus.
9. Procédé selon l’une des revendications 1 à 7, caractérisé en ce qu’on choisit ledit deuxième matériau avec une proportion en masse de phosphore inférieure ou égale à 15%. 9. Method according to one of claims 1 to 7, characterized in that said second material is chosen with a mass proportion of phosphorus less than or equal to 15%.
10. Procédé selon la revendication 9, caractérisé en ce qu’on choisit ledit deuxième matériau avec une proportion en masse de phosphore comprise entre 6% et 12%. 10. Method according to claim 9, characterized in that said second material is chosen with a mass proportion of phosphorus of between 6% and 12%.
11. Procédé selon la revendication 9, caractérisé en ce qu’on choisit ledit deuxième matériau avec une proportion en masse de phosphore comprise entre 1 % et 6%. 11. Method according to claim 9, characterized in that said second material is chosen with a mass proportion of phosphorus of between 1% and 6%.
12. Procédé selon la revendication 9, caractérisé en ce qu’on choisit ledit deuxième matériau avec une proportion en masse de phosphore inférieure ou égale à 1 %. 12. Method according to claim 9, characterized in that said second material is chosen with a mass proportion of phosphorus less than or equal to 1%.
13. Procédé selon l’une des revendications 1 à 7, caractérisé en ce qu’on choisit ledit deuxième matériau comportant du bore. 13. Method according to one of claims 1 to 7, characterized in that said second material comprising boron is chosen.
14. Procédé selon l’une des revendications 1 à 7, caractérisé en ce qu’on choisit ledit deuxième matériau constitué uniquement de nickel et de bore. 14. Method according to one of claims 1 to 7, characterized in that said second material is chosen consisting solely of nickel and boron.
15. Procédé selon l’une des revendications 1 à 7, caractérisé en ce qu’on choisit ledit deuxième matériau amagnétique avec une proportion en masse de phosphore comprise entre 10% et 15%. 15. Method according to one of claims 1 to 7, characterized in that said second non-magnetic material is chosen with a proportion by mass of phosphorus of between 10% and 15%.
16. Procédé selon l’une des revendications 1 à 15, caractérisé en ce qu’on applique ledit deuxième matériau avec une épaisseur inférieure à 10 micromètres. 16. Method according to one of claims 1 to 15, characterized in that said second material is applied with a thickness of less than 10 micrometers.
17. Procédé selon la revendication 16, caractérisé en ce qu’on applique ledit deuxième matériau avec une épaisseur inférieure à 5 micromètres. 17. Method according to claim 16, characterized in that said second material is applied with a thickness of less than 5 micrometers.
18. Procédé selon la revendication 17, caractérisé en ce qu’on applique ledit deuxième matériau avec une épaisseur comprise entre 0.2 micromètre et 5.0 micromètre. 18. Method according to claim 17, characterized in that said second material is applied with a thickness of between 0.2 micrometer and 5.0 micrometer.
19. Procédé selon la revendication 18, caractérisé en ce qu’on applique ledit deuxième matériau avec une épaisseur comprise entre 0.2 micromètre et 2.0 micromètre. - 11 - 19. Method according to claim 18, characterized in that said second material is applied with a thickness of between 0.2 micrometer and 2.0 micrometer. - 11 -
20. Procédé selon l’une des revendications 1 à 19, caractérisé en ce qu’on applique un traitement thermique à l’ensemble formé par ledit substrat et son dit revêtement, à une température comprise entre 100°C et 500°C, pendant 1 à 8 heures. 20. Method according to one of claims 1 to 19, characterized in that a heat treatment is applied to the assembly formed by said substrate and its said coating, at a temperature between 100°C and 500°C, for 1 to 8 hours.
21. Procédé selon la revendication 20, caractérisé en ce qu’on effectue ledit traitement thermique après l’opération de revêtement. 21. Method according to claim 20, characterized in that said heat treatment is carried out after the coating operation.
22. Procédé selon la revendication 20, caractérisé en ce qu’on effectue ledit traitement thermique avant l’opération de revêtement. 22. Method according to claim 20, characterized in that said heat treatment is carried out before the coating operation.
23. Procédé selon l’une des revendications 1 à 22, caractérisé en ce qu’on réalise ledit substrat par un procédé « LIGA ». 23. Method according to one of claims 1 to 22, characterized in that said substrate is produced by a “LIGA” process.
24. Procédé selon l’une des revendications 1 à 23, caractérisé en ce qu’on applique ledit procédé à la fabrication d’un mobile d’échappement qui est une roue d’échappement ou une ancre. 24. Method according to one of claims 1 to 23, characterized in that said method is applied to the manufacture of an escapement wheel which is an escapement wheel or an anchor.
25. Procédé selon la revendication 2 et l’une des revendications 1 à 24, caractérisé en ce qu’on limite l’épaisseur dudit deuxième matériau qui constitue la couche périphérique dudit mobile au niveau de ladite au moins une surface jouxtant une surface frottante à moins de 10 micromètres. 25. Method according to claim 2 and one of claims 1 to 24, characterized in that the thickness of said second material which constitutes the peripheral layer of said mobile at the level of said at least one surface adjoining a friction surface is limited to less than 10 micrometers.
26. Procédé selon la revendication 24, caractérisé en ce qu’on limite l’épaisseur dudit deuxième matériau qui constitue la couche périphérique dudit mobile au niveau de ladite au moins une surface jouxtant une surface frottante à moins de 5 micromètres. 26. Method according to claim 24, characterized in that the thickness of said second material which constitutes the peripheral layer of said mobile at the level of said at least one surface adjoining a friction surface is limited to less than 5 micrometers.
EP21769741.6A 2020-09-15 2021-08-31 Method for manufacturing a micromechanical component, in particular a timepiece mobile having an optimised surface Pending EP4214581A1 (en)

Applications Claiming Priority (2)

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EP20196228.9A EP3968095A1 (en) 2020-09-15 2020-09-15 Method for manufacturing a micromechanical component, in particular of a timepiece mobile, with optimised contact surface
PCT/EP2021/074027 WO2022058160A1 (en) 2020-09-15 2021-08-31 Method for manufacturing a micromechanical component, in particular a timepiece mobile having an optimised surface

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US (1) US20230288872A1 (en)
EP (2) EP3968095A1 (en)
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CH1060769A4 (en) * 1969-07-11 1971-07-15
EP2082014B1 (en) * 2006-11-02 2018-02-14 Rolex Sa Watch
EP2586879A1 (en) * 2011-10-27 2013-05-01 Nivarox-FAR S.A. Method for thermal treatment of micromechanical clock parts
EP3171230B1 (en) * 2015-11-19 2019-02-27 Nivarox-FAR S.A. Timepiece component with improved tribology
EP3171229A1 (en) * 2015-11-19 2017-05-24 Nivarox-FAR S.A. Clock component
EP3390696B1 (en) * 2015-12-18 2023-01-04 Rolex S.A. Method for manufacturing a clock component
EP3273307A1 (en) * 2016-07-19 2018-01-24 Nivarox-FAR S.A. Part for clock movement
CH712719B1 (en) * 2016-07-19 2020-12-15 Nivarox Sa Watch component for watch movement.
CH712718B1 (en) * 2016-07-19 2020-12-15 Nivarox Sa Pivot pin for clockwork movement.
EP3273306A1 (en) * 2016-07-19 2018-01-24 Nivarox-FAR S.A. Part for clock movement

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KR20230044271A (en) 2023-04-03
EP3968095A1 (en) 2022-03-16
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CN116075781A (en) 2023-05-05
JP2023534523A (en) 2023-08-09

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