EP3543796A1 - Verfahren zur herstellung einer siliziumfeder - Google Patents

Verfahren zur herstellung einer siliziumfeder Download PDF

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Publication number
EP3543796A1
EP3543796A1 EP18163053.4A EP18163053A EP3543796A1 EP 3543796 A1 EP3543796 A1 EP 3543796A1 EP 18163053 A EP18163053 A EP 18163053A EP 3543796 A1 EP3543796 A1 EP 3543796A1
Authority
EP
European Patent Office
Prior art keywords
hairspring
silicon
layer
spiral
etching
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.)
Withdrawn
Application number
EP18163053.4A
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English (en)
French (fr)
Inventor
Pierre Cusin
Marco Verardo
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.)
Nivarox Far SA
Nivarox SA
Original Assignee
Nivarox Far SA
Nivarox SA
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 Nivarox Far SA, Nivarox SA filed Critical Nivarox Far SA
Priority to EP18163053.4A priority Critical patent/EP3543796A1/de
Priority to KR1020207026526A priority patent/KR102448668B1/ko
Priority to JP2020549548A priority patent/JP7100711B2/ja
Priority to US16/982,418 priority patent/US11300926B2/en
Priority to EP19712197.3A priority patent/EP3769160A1/de
Priority to PCT/EP2019/057160 priority patent/WO2019180177A1/fr
Priority to CN201980017845.2A priority patent/CN111819501A/zh
Publication of EP3543796A1 publication Critical patent/EP3543796A1/de
Withdrawn legal-status Critical Current

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    • 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
    • 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
    • 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
    • G04B17/26—Compensation of mechanisms for stabilising frequency for the effect of variations of the impulses

Definitions

  • the invention relates to a method of manufacturing a silicon spiral and, more specifically, such a spiral used as a compensating spring cooperating with a known balance of inertia to form a resonator having a predetermined frequency.
  • the step of etching several spirals in a silicon wafer offers a non-negligible geometrical dispersion between the spirals of the same wafer and a greater dispersion between spirals of two wafers etched at different times.
  • the stiffness of each spiral engraved with the same engraving pattern is variable by creating significant manufacturing dispersions.
  • the object of the present invention is to overcome all or part of the disadvantages mentioned above by proposing a method of manufacturing a spiral whose dimensions are sufficiently precise not to require retouching.
  • a compensating balance spring is thus obtained which, advantageously according to the invention, comprises a silicon-based core and a coating based on silicon oxide.
  • the compensating hairspring thus has a very high dimensional accuracy and, incidentally, a thermal compensation of the whole resonator very fine.
  • the invention relates to a compensating hairspring 1 visible at the figure 2a and its manufacturing process to ensure a very high dimensional accuracy of the spiral and, incidentally, to ensure a more precise stiffness of said spiral.
  • the compensating spiral 1 is formed based on a material, optionally coated with a thermal compensation layer, and intended to cooperate with a known inertia balance.
  • the silicon-based material used as a compensating spiral may be monocrystalline silicon whatever its crystalline orientation, doped monocrystalline silicon whatever its crystalline orientation, amorphous silicon, porous silicon, polycrystalline silicon, silicon nitride, silicon carbide, quartz regardless of its crystalline orientation or the oxide of silicon.
  • monocrystalline silicon whatever its crystalline orientation
  • doped monocrystalline silicon whatever its crystalline orientation
  • amorphous silicon porous silicon
  • polycrystalline silicon silicon
  • silicon nitride silicon carbide
  • quartz regardless of its crystalline orientation or the oxide of silicon.
  • other materials can be envisioned as a glass, a ceramic, a cermet, a metal or a metal alloy.
  • the explanation below will be focused on a silicon-based material.
  • Each type of material may be surface-modified or layer-coated to thermally compensate for the base material as explained above.
  • the invention relates to a method of manufacturing a silicon spiral 1 visible at the figure 3 .
  • the process steps represent only a median section along the line A of a single silicon balance spring 1 formed in the wafer 10 of the figure 1 , the number of turns 3 of the spiral 1 being reduced to facilitate the reading of the figures.
  • the method comprises, as illustrated in figure 3 a first step a) consisting in providing SOI wafers 10, that is to say composed of two silicon layers 11 and 12, bonded to one another by a silicon oxide layer 13 Each of these three layers has one or more specific roles.
  • the lower layer of silicon 12, called “handle”, serves essentially as mechanical support, so as to perform the process on a sufficiently rigid assembly (which the reduced thickness of the "device” is not able to guarantee) . It is also formed of a monocrystalline silicon plate, generally of a similar orientation to the "device" layer.
  • the oxide layer 13 intimately bonds the two silicon layers 11 and 12. In addition, it will also serve as a stop layer for subsequent operations.
  • the following step b) consists in growing on the surface of the wafer (s) 10 a layer of silicon oxide, exposing the wafer or wafers to an oxidizing atmosphere at high temperature.
  • the layer varies according to the thickness of the "device" to be structured. It is typically between 1 and 4 ⁇ m.
  • step d the areas exposed or on the contrary coated with resin are then exploited.
  • a first etching process makes it possible to transfer the patterns defined in the resin in the preceding steps to the previously grown silicon oxide.
  • silicon oxide is structured by a plasma dry etching, directional and reproducing the quality of the flanks of the resin serving as a mask for this operation.
  • the silicon surface of the upper layer 11 is then exposed and ready for a DRIE etching.
  • the resin can be preserved or not depending on whether it is desired to use the resin as a mask during the DRIE etching.
  • Silicon exposed and unprotected by silicon oxide is etched in a direction perpendicular to the surface of the wafer (Bosch® DRIE anisotropic etching).
  • the patterns formed first in the resin, then in the silicon oxide, are "projected” into the thickness of the "device” layer 11.
  • the etching opens on the silicon oxide layer 13 bonding the two silicon layers 11 and 12, the etching stops. Indeed, like the silicon oxide serving as a mask during the Bosch® process and resistant to etching itself, the buried oxide layer 13, of the same nature, also resists therein.
  • the "device" silicon layer 11 is then structured throughout its thickness by the defined patterns representing the components to be manufactured, now revealed by this DRIE etching, namely a spiral 1 comprising turns 3 and a ferrule 2.
  • the components remain integral with the "handle" layer 12 to which they are bonded by the buried silicon oxide layer 13.
  • step e) could equally well be obtained by chemical etching in the same silicon-based material.
  • step e several spirals can be formed in the same wafer in dimensions larger than the dimensions necessary to obtain several spirals of an initial stiffness or several spirals of several initial stiffnesses.
  • step e) the residues of the passivation resin resulting from the Bosch® process are then removed, and the oxide having served as a mask for the DRIE etching is removed in solution. aqueous hydrofluoric acid.
  • a layer of silicon oxide is again grown on the surface of the silicon (around the "device” 11 and “handle” layers 12), this oxide layer will serve as a protection for the components during the operation to release them by separating them from the "handle” layer 12.
  • a second photolithography operation similar to the first carried out in step c) is carried out on the back of the wafer 10 (hence on the "handle" layer 12). To do this the wafer 10 is returned, the resin is deposited therein and then exposed through a mask.
  • the area of the exposed resin is then removed by means of a solvent, revealing the previously formed oxide layer, which is then structured via dry etching.
  • a complete etching of the exposed "handle" layer 12 is carried out using an aqueous solution, based on potassium hydroxide (KOH), tetramethylammonium hydroxide, or DRIE engraving.
  • KOH potassium hydroxide
  • tetramethylammonium hydroxide or DRIE engraving.
  • step g1) to completely release the components, the various silicon oxide layers are then etched by wet etching with a hydrofluoric acid solution.
  • the spirals 1 formed are held at a frame via at least one fastener, the frame and the fasteners having been formed at the same time as the spirals during the step e) of etching DRIE.
  • the method comprises a step h) intended to determine the initial stiffness of the hairspring.
  • a step h) can be carried out directly on the hairspring still attached to the wafer 10 or on the whole or on a sample of the spirals still attached to the wafer or on a spiral detached from the wafer.
  • step h) comprises a first phase h1) intended to measure the frequency of an assembly comprising the hairspring coupled with a balance having a known inertia and then to deduce the initial stiffness of the hairspring.
  • the oscillation frequency of the sprung balance assembly makes it possible to determine the angular stiffness of the spiral tested, and thereby the precise dimensions of the turn section 3 of the spiral spring 1 (its thickness mainly, the height being known , since this is the thickness of the "device" layer of the base substrate).
  • Such a measurement phase can in particular be dynamic and carried out according to the teachings of the document EP 2 423 764 , incorporated by reference into the present application.
  • a static method carried out according to the teachings of the document EP 2 423 764 can also be used to determine the stiffness of the hairspring.
  • step h) may also consist of a determination of the average initial stiffness of a representative sample or the set of spirals formed on the same wafer.
  • the turn dimensions to be obtained are calculated to obtain the overall dimensions necessary to obtain said hairspring of a desired stiffness (or final stiffness).
  • the process continues with a sequence for removing the excess material from the hairspring to the necessary dimensions to obtain the hairspring of final stiffness.
  • Step i) is to oxidize the hairspring in order to convert said thickness of silicon-based material to silicon dioxide and thereby form an oxidized hairspring.
  • a phase may, for example, be obtained by thermal oxidation.
  • thermal oxidation can, for example, be carried out between 800 and 1200 ° C under an oxidizing atmosphere using water vapor or oxygen gas to form silicon oxide on the spiral.
  • the silicon oxide grows regularly, the oxidation rate and the resulting thickness are perfectly mastered by those skilled in the art which ensures uniformity of the oxide layer.
  • Step i) is continued with a step j) intended to remove the oxide of the spiral making it possible to obtain a silicon-based spiral with the overall dimensions necessary to obtain the final stiffness.
  • a step is obtained by a chemical etching.
  • Such chemical etching can be carried out, for example, by means of a solution based on hydrofluoric acid for removing silicon oxide from the spiral.
  • Steps i) and j) make it possible to bring the dimensions of the turn 3 to intermediate values determined during the calculation step h2).
  • step k) consists in oxidizing the hairspring again to coat it with a layer of silicon dioxide in order to form a hairspring 1 which is thermally compensated.
  • a step may, for example, be obtained by thermal oxidation.
  • thermal oxidation can, for example, be carried out between 800 and 1200 ° C under an oxidizing atmosphere using water vapor or oxygen gas to form silicon oxide on the spiral.
  • FIGS. Figures 2a and 2b which, advantageously according to the invention, comprises a core 30 based on silicon and a coating 31 based on silicon oxide.
  • This second oxidation makes it possible to adjust both the mechanical (stiffness) and thermal (temperature compensation) performance of the future hairspring 1.
  • the dimensions of the turn 3 satisfy the requirement of angular stiffness sought and the layer silicon oxide increases the stiffness according to the dimensional change of the balance / hairspring depending on the temperature.
  • the method may also comprise a metallization step I). Indeed, the growth of a non-negligible layer of silicon oxide on the surface of the spirals does not bring only advantages. This layer traps and fixes electrical charges, which will lead to phenomena of electrostatic bonding either with the spiral environment, or turns between them.
  • This layer also has hydrophilic properties, and it is known that the absorption of moisture causes a drift of the stiffness of the hairspring and therefore the running of the watch.
  • a thin layer of a metal such as chromium, titanium, tantalum or one of their alloys renders both the surface of the hairspring 1 waterproof and conductive, eliminating the effects mentioned above.
  • a metal such as chromium, titanium, tantalum or one of their alloys renders both the surface of the hairspring 1 waterproof and conductive, eliminating the effects mentioned above.
  • Such a layer can be obtained according to the teachings of the document EP 2,920,653 , incorporated by reference into the present application.
  • This thin layer is chosen as thin as possible so as not to disturb the performance adjusted above. Adequate heat treatment ensures good adhesion of the thin layer.
  • the method may also comprise step I) intended to separate the spirals 1 of the wafer 10 and to assemble them with a known balance of inertia to form a balance-spring resonator which is compensated thermally or otherwise, it is that is, whose frequency is sensitive or not to temperature variations.
  • the balance even if it comprises a predefined construction inertia, may comprise movable weights to provide a setting parameter before or after the sale of the timepiece.
EP18163053.4A 2018-03-21 2018-03-21 Verfahren zur herstellung einer siliziumfeder Withdrawn EP3543796A1 (de)

Priority Applications (7)

Application Number Priority Date Filing Date Title
EP18163053.4A EP3543796A1 (de) 2018-03-21 2018-03-21 Verfahren zur herstellung einer siliziumfeder
KR1020207026526A KR102448668B1 (ko) 2018-03-21 2019-03-21 실리콘 헤어스프링을 제조하기 위한 방법
JP2020549548A JP7100711B2 (ja) 2018-03-21 2019-03-21 ケイ素ひげぜんまいを製造する方法
US16/982,418 US11300926B2 (en) 2018-03-21 2019-03-21 Process for fabricating a silicon hairspring
EP19712197.3A EP3769160A1 (de) 2018-03-21 2019-03-21 Verfahren zur herstellung einer siliciumhaarfeder
PCT/EP2019/057160 WO2019180177A1 (fr) 2018-03-21 2019-03-21 Procede de fabrication d'un spiral en silicium
CN201980017845.2A CN111819501A (zh) 2018-03-21 2019-03-21 制造硅游丝的方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP18163053.4A EP3543796A1 (de) 2018-03-21 2018-03-21 Verfahren zur herstellung einer siliziumfeder

Publications (1)

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EP3543796A1 true EP3543796A1 (de) 2019-09-25

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EP18163053.4A Withdrawn EP3543796A1 (de) 2018-03-21 2018-03-21 Verfahren zur herstellung einer siliziumfeder
EP19712197.3A Pending EP3769160A1 (de) 2018-03-21 2019-03-21 Verfahren zur herstellung einer siliciumhaarfeder

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EP19712197.3A Pending EP3769160A1 (de) 2018-03-21 2019-03-21 Verfahren zur herstellung einer siliciumhaarfeder

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US (1) US11300926B2 (de)
EP (2) EP3543796A1 (de)
JP (1) JP7100711B2 (de)
KR (1) KR102448668B1 (de)
CN (1) CN111819501A (de)
WO (1) WO2019180177A1 (de)

Cited By (2)

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CH716603A1 (fr) * 2019-09-16 2021-03-31 Sigatec Sa Procédé de fabrication de spiraux horlogers.
EP3882714A1 (de) * 2020-03-19 2021-09-22 Patek Philippe SA Genève Verfahren zur herstellung einer uhrenkomponente aus silizium

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CH716605A1 (fr) * 2019-09-16 2021-03-31 Richemont Int Sa Procédé de fabrication d'une pluralité de résonateurs sur une plaquette.
EP3907565A1 (de) 2020-05-07 2021-11-10 Patek Philippe SA Genève Verfahren zur herstellung einer uhrenkomponente aus silizium
EP4312084A1 (de) 2022-07-26 2024-01-31 Nivarox-FAR S.A. Verfahren zur herstellung einer siliziumspirale
EP4332686A1 (de) 2022-08-30 2024-03-06 ETA SA Manufacture Horlogère Suisse Spiralfeder für eine spiralunruh-einheit einer uhrwerke

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EP1422436A1 (de) 2002-11-25 2004-05-26 CSEM Centre Suisse d'Electronique et de Microtechnique SA Spiraluhrwerkfeder und Verfahren zu deren Herstellung
EP2423764A1 (de) 2010-08-31 2012-02-29 Rolex S.A. Vorrichtung zum Messen des Drehmomentes einer Spirale
EP2920653A1 (de) 2012-11-16 2015-09-23 Nivarox-FAR S.A. Resonator mit geringerer empfindlichkeit gegenüber klimatischen schwankungen
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CH716603A1 (fr) * 2019-09-16 2021-03-31 Sigatec Sa Procédé de fabrication de spiraux horlogers.
EP3845770A1 (de) * 2019-09-16 2021-07-07 Sigatec SA Verfahren zur herstellung von uhrwerk-spiralfedern
EP3915788A1 (de) * 2019-09-16 2021-12-01 Sigatec SA Verfahren zur herstellung eines loses von uhrwerk-spiralfedern
EP3882714A1 (de) * 2020-03-19 2021-09-22 Patek Philippe SA Genève Verfahren zur herstellung einer uhrenkomponente aus silizium
WO2021186333A1 (fr) * 2020-03-19 2021-09-23 Patek Philippe Sa Geneve Procede de fabrication d'un composant horloger en silicium

Also Published As

Publication number Publication date
KR102448668B1 (ko) 2022-09-28
CN111819501A (zh) 2020-10-23
WO2019180177A1 (fr) 2019-09-26
JP7100711B2 (ja) 2022-07-13
US20210080909A1 (en) 2021-03-18
JP2021535356A (ja) 2021-12-16
KR20200120949A (ko) 2020-10-22
US11300926B2 (en) 2022-04-12
EP3769160A1 (de) 2021-01-27

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