EP3764169A1 - Verfahren zum abschnittsweisen satinieren einer uhrenkomponente aus silizium - Google Patents

Verfahren zum abschnittsweisen satinieren einer uhrenkomponente aus silizium Download PDF

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Publication number
EP3764169A1
EP3764169A1 EP19185364.7A EP19185364A EP3764169A1 EP 3764169 A1 EP3764169 A1 EP 3764169A1 EP 19185364 A EP19185364 A EP 19185364A EP 3764169 A1 EP3764169 A1 EP 3764169A1
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EP
European Patent Office
Prior art keywords
etching
silicon
sacrificial layer
silicon surface
layer
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.)
Granted
Application number
EP19185364.7A
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English (en)
French (fr)
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EP3764169B1 (de
Inventor
Rémy FOURNIER
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.)
Patek Philippe SA Geneve
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Patek Philippe SA Geneve
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Priority to EP19185364.7A priority Critical patent/EP3764169B1/de
Publication of EP3764169A1 publication Critical patent/EP3764169A1/de
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Publication of EP3764169B1 publication Critical patent/EP3764169B1/de
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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
    • G04B19/00—Indicating the time by visual means
    • G04B19/04—Hands; Discs with a single mark or the like
    • G04B19/042—Construction and manufacture of the hands; arrangements for increasing reading accuracy
    • 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
    • G04B13/00—Gearwork
    • G04B13/02—Wheels; Pinions; Spindles; Pivots
    • 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
    • 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
    • G04B19/00—Indicating the time by visual means
    • G04B19/06—Dials
    • G04B19/12—Selection of materials for dials or graduations markings
    • G—PHYSICS
    • G04—HOROLOGY
    • G04D—APPARATUS OR TOOLS SPECIALLY DESIGNED FOR MAKING OR MAINTAINING CLOCKS OR WATCHES
    • G04D3/00—Watchmakers' or watch-repairers' machines or tools for working materials
    • G04D3/0074—Watchmakers' or watch-repairers' machines or tools for working materials for treatment of the material, e.g. surface treatment

Definitions

  • the present invention relates to a method for spot-etching a silicon surface. It relates more particularly to a process for spot-etching a silicon surface of a wafer in which a timepiece component is then micromachined or, alternatively, for spot-etching a silicon surface of the watch component itself or of the watch component itself. 'draft of it.
  • to roughen is used to mean attacking a surface so as to remove its "polish”.
  • a surface is thus qualified as “frosted” when it has sufficient roughness to diffuse or absorb the incident light.
  • a surface is said to be rough when it presents an irregular relief comprising hollows and peaks, these hollows, or craters, having a depth ranging from a hundred nanometers to one micrometer.
  • Crystalline silicon is opaque and reflects light. Its appearance is that of a dark gray metal. This color can give a somewhat austere appearance to parts made of silicon.
  • An aim of the present invention is to remedy the problems of the prior art which have just been explained.
  • the present invention achieves this and other object by providing a method for spot-etching a silicon surface, which is in accordance with claim 1 appended hereto.
  • step (a) of the method of the invention the locations of the silicon surface which will be etched by making an etching mask comprising apertures are first of all defined.
  • a sacrificial layer of resin is deposited on the etching mask and inside its openings.
  • the production of the sacrificial layer does not involve either exposure or annealing of the resin of the sacrificial layer.
  • One advantage of this feature is that it contributes to shortening and simplifying the implementation of step (b) of the method.
  • the layer of sacrificial resin is then attacked by deep reactive ionic etching (usually designated by its acronym "DRIE"), so as to transfer inhomogeneities of the sacrificial layer. on the places to be roughened of the silicon surface.
  • DRIE deep reactive ionic etching
  • Deep reactive ion etching is the most widely used etching technique for the micromachining of silicon-based components. This technique is already described in particular in the patent document WO 94/14187 on behalf of Robert Bosch GmbH. This document is incorporated by reference in the present description.
  • Deep reactive ion etching enables the etching of almost vertical flank profiles in a silicon-based substrate by applying a procedure that alternates the steps of depositing an inert passivation layer and plasma etching.
  • the stages of deposition of the passivation layer and those of etching all involve fluorinated compounds, so that they take place in the same chemical context.
  • Each step lasts a few seconds, the passivation layer is formed over the entire surface of the substrate, so that the latter is protected against any subsequent etching.
  • the deep reactive ionic etching which takes place in step (c) of the method of the invention, is distinguished from other common etching methods by its highly anisotropic, almost unidirectional character.
  • One advantage of using the deep reactive ionic etching technique is therefore that it allows the inhomogeneities of the sacrificial layer to be transferred to the substrate with high resolution and without attenuation. It is important to note that this advantage is not found with other current techniques which have a lower degree of anisotropy. Indeed, with these less anisotropic techniques, the considerable divergence that exists between the directions of etching only allows the transfer of a strongly attenuated roughness onto the silicon surface.
  • the various embodiments of the invention make it possible to roughen in places, in identical or different ways, the surface of a silicon wafer in which we will then micro- to machine a watch component or, alternatively, to roughen in places a surface, or more surfaces, of said watch component itself or of the blank thereof.
  • the wafer, the watch component, or its blank may or may not have been covered beforehand with a layer of SiO 2 .
  • the invention makes it possible to combine on the same plate, blank or component, two different effects, such as matt and gloss or polished and frosted, which offers new possibilities in the covering.
  • the surfaces frosted in places correspond to surfaces visible from the outside of the timepiece.
  • the frosted surfaces are also preferably located in non-functional areas of the watch components, so as not to interfere with the watch mechanisms and to maintain optimum mechanical properties.
  • FIG. 1 illustrates an object (referenced 2) which comprises at least one silicon surface 4 which it is desired to roughen in places using the method of the invention.
  • object denotes a silicon wafer. It will be understood, however, that in accordance with other variants (not illustrated), this term could alternatively designate a watch component based on silicon or the blank of such a component.
  • the figure 2 illustrates the object 2 following the production by photolithography of a perforated etching mask 6 on the silicon surface 4.
  • This mask 6 can be produced in any manner known to those skilled in the art. In particular by first depositing a layer of photosensitive resin on the surface 4, and then structuring this layer by photolithography before subjecting it to annealing.
  • the photosensitive resin layer is a layer of AZ® 9260, the thickness of which is approximately 7 microns. It will be understood, however, that the resin can naturally be of another type. In addition, its thickness is obviously not necessarily 7 microns. The thickness of the resin layer is typically, but not necessarily, between 5 and 15 microns.
  • the figure 3 illustrates object 2 following the deposition of a sacrificial layer 8 of resin on the etching mask 6 and on the parts of the surface 4 which are exposed through the openings of the mask 6.
  • the sacrificial layer of resin generally has a thickness less than or equal to 5 microns, typically less than or equal to 3 microns.
  • the sacrificial layer 8 is made with positive photosensitive resin of the AZ® 1518 type. This particular resin is suitable for making thin layers.
  • the resin can be applied with a spinner at 5000 rpm. This speed leads to the deposition of a thin layer, the thickness of which is approximately 1.8 microns.
  • the resin which forms the sacrificial layer 8 has been deposited, one passes to the subsequent etching step without having exposed or annealed the resin layer 8 beforehand.
  • the figure 4 illustrates the object 2 after the aforementioned etching step.
  • This etching step consists of attacking the layer of sacrificial resin 8 by Deep Reactive Ion Etching (DRIE).
  • DRIE Deep Reactive Ion Etching Table I below indicates the main parameters used in the present example to implement the DRIE etching.
  • the version of the DRIE process used in the present example is based on a cycle consisting of a step (designated by the acronym DEP) of forming a passivation layer, followed by two distinct steps (respectively designated by E1 and E2) plasma etching.
  • DEP step
  • E1 and E2 two distinct steps
  • a gas mixture formed of 4/5 of C 4 F 8 and 1/5 of O 2 is injected.
  • a first plasma produced from SF 6 is used for the first etching step E1.
  • the function of this first plasma is to disintegrate the part of the passivation layer which is at the bottom of the profiles.
  • the second etching step E2 uses a plasma formed from a mixture of SF 6 and C 4 F 8 .
  • the function of this second plasma is to hollow out the profiles by reactive etching of the bottom of the latter.
  • the DRIE etching step continues long enough to transfer inhomogeneities of the sacrificial layer 8 to the places to be roughened (or in other words rough) of the silicon surface 4. It is possible to It will therefore be understood that the etching continues at a minimum until through openings have been created through the sacrificial layer 8.
  • This first hinge moment can for example be identified by detecting the presence of silicon atoms, or of compounds. comprising silicon, in the reactor in which the DRIE etching is carried out. At the other extreme, the etching should not be continued after the sacrificial layer 8 has been completely consumed.
  • this second pivotal moment is concomitant with the disappearance of the chemical species characteristic of the sacrificial layer, which were present until then in the reactor.
  • a person skilled in the art After calibrating the process, a person skilled in the art will be able to determine, for example by timing, the moment when he wishes to stop the etching. The moment that a person skilled in the art will choose for stopping the etching will be situated in the interval between the aforementioned first and second pivotal moments.
  • the figure 5 illustrates the object 2 following a last step consisting in removing the etching mask 6, the resin residues from the sacrificial layer 8, as well as other residues left by the passivation steps.
  • the removal of the resin and of the C 4 F 8 residues is carried out using an O 2 plasma.
  • the silicon surface which is desired to be roughened by applying the method is the surface of a wafer (referenced 12). It will however be understood that according to other variants (not illustrated) of this second embodiment, the surface in question could be that of a silicon-based watch component or that of the blank of such a component. .
  • the silicon body of wafer 12 is coated on all sides with a layer of silicon dioxide (SiO 2 ) 15, the thickness of which is approximately 0.8 microns.
  • the layer 15 may for example have been formed on the wafer 12 by thermal oxidation of the silicon at a temperature between 900 ° C and 1200 ° C.
  • the figure 6 illustrates the wafer 12 after a first step consisting in the production by photolithography of an openwork etching mask 16 on the upper face of the wafer 12.
  • the etching mask is a resin mask, and it can be produced conventionally, for example with photosensitive resin of the AZ® 1518 type.
  • the resin can be applied with a spinner at 4000 revolutions / minute so as to deposit a layer whose thickness is approximately 2.6 microns.
  • the resin layer deposited by photolithography is then structured before subjecting it to annealing.
  • the step whose result is illustrated in figure 7 consists in etching the SiO 2 layer through the openings of the resin mask 16, so as to structure it and make it an etching mask.
  • RIE reactive ion etching
  • the figure 8 illustrates wafer 12 after removal of resin mask 16. This removal can be done in a number of ways known to those skilled in the art, and it will be further understood that it could just as well occur later in the process.
  • the oxide layer 15 which had been structured during the previous step is now in the position of serving as an etching mask capable of withstanding the DRIE process which will be implemented during a subsequent step.
  • the figure 8 also shows a new sacrificial layer (referenced 18) which covers the etching mask 15 in SiO 2 , as well as the silicon exposed through the openings of the mask 15.
  • the sacrificial layer 18 can be made with AZ® 1518 type resin.
  • the resin can be applied with a spinner. 5000 revolutions / minute, so as to form a thin layer, the thickness of which is approximately 1.8 microns.
  • the etching step aims to create inhomogeneities in the sacrificial layer 18 and to transfer the latter to the places of the silicon surface which it is desired to make rough.
  • This step can be implemented in an identical manner to what has already been explained above in relation to the figure 4 of the first example.
  • the DRIE etching step continues long enough to transfer inhomogeneities of the sacrificial layer 18 to the places to be roughened of the silicon surface, so that said places are roughened according to the degree of desired frosting.
  • the figure 10 illustrates wafer 12 after the resin residues of the sacrificial layer 18 and the residues of C 4 F 8 left by the passivation steps have been removed.
  • the elimination of residues can be carried out using an 02 plasma.
  • the process step, the result of which is illustrated in figure 11 consists in the elimination of all the SiO 2 which covers the wafer 12. In a manner known not per se, this step can be carried out in the form of wet etching with BHF.
  • the figure 12 is a photographic view showing the upper face of a silicon wafer, the surface of which has been roughened in places by applying one or the other of the two exemplary embodiments of the invention which have been described so far .
  • the areas of the silicon surface which have been etched by the process are clearly visible in the photograph.
  • a review of the figure 12 allows one to get an idea of the innumerable graphic possibilities offered by the method of the invention for giving watchmaking components (eg, balance springs, hands, anchors, wheels, dials, etc.) a visually unique personality.
  • FIG. 13 illustrates the wafer 12, the silicon surface of which has previously been frosted in places in accordance with the second embodiment which has been described above.
  • the figure 13 illustrates the wafer 12 following the formation of a new openwork etching mask 20 on its upper face.
  • This new mask 20 can be produced in a conventional manner, for example by first depositing a layer of approximately 7 microns thick of AZ® 9260 photosensitive resin.
  • the mask of etching 20 must be capable of withstanding the DRIE process which will be implemented in a subsequent step.
  • the figure 14 shows wafer 12 after performing DRIE etching to cut wafer 12 into several pieces. It is worth clarifying that the cutting of a wafer by DRIE engraving is already known as such. Traditional settings are moreover preferably used for carrying out this etching. It will be understood that at least some of the pieces represented schematically in the figure 14 , are in fact horological components or at least blanks of such components.
  • the figures 13 and 14 describe the etching of a face of a wafer by DRIE after the surface of the latter has been frosted in places using the method of the invention.
  • An embodiment of the invention will now be described in which, conversely, at least one timepiece component blank (in this case the blank of a hairspring) is first cut from a wafer. before roughening the surface of the component in places.
  • This third exemplary embodiment of the method of the invention will be described with reference to the figures 20 to 23 appended, which are diagrammatic views in vertical section which illustrate the blank of a silicon watch component at four successive instants of the implementation of a method.
  • the figures 17 to 19 are schematic views in vertical section which constitute three successive snapshots showing the production of the blank of a silicon watch component from an SOI wafer.
  • the figure 17 illustrates the wafer SOI (silicon on insulator) referenced 22. Conventionally, this wafer is made up of two layers of silicon and a layer of silicon dioxide sandwiched between the layers of silicon.
  • the figure 17 illustrates the wafer 22 following the production of an openwork etching mask 26 by photolithography on the upper face of the wafer 22.
  • the mask 26 can be produced in a conventional manner. For example, by proceeding in the manner described above in relation to the figure 13 .
  • the figure 18 illustrates the SOI 22 wafer after the upper silicon layer has been etched over its entire thickness (approximately 120 microns) by conventional DRIE etching.
  • the figure 19 illustrates the SOI wafer 22 after the removal of the etching mask 26.
  • the dissolution of the mask 26 can be obtained for example by immersing the SOI wafer 22 for a few hours in a KOH solution.
  • the figure 19 further shows that a layer of silicon dioxide 24 entirely covers the surfaces of the SOI wafer 22 and of the timepiece component blank which is formed in its upper silicon layer.
  • the thickness of the SiO 2 layer is approximately 0.8 microns. It will be understood that the dioxide layer 24 has been formed after the removal of the etching mask 26.
  • the dioxide layer may have been formed on the wafer 22, for example, by thermal oxidation at a temperature between 900 ° C and 1200 ° C.
  • the figures 20 to 23 are schematic vertical sectional views illustrating four successive instants of the third exemplary particular embodiment of the invention.
  • this third embodiment makes it possible to roughen in places the surface of a watch component or of the blank of such a component; the component or blank having first been cut in a wafer.
  • the method is implemented to roughen at least in places the blank of the watch component whose production by micro-machining of the SOI wafer (referenced 22) has just been described in relation to the components.
  • figures 17 to 19 The figure 20 illustrates the SOI 22 wafer, as well as the watch component blank which is formed in the top layer of the latter, after having removed the part of the silicon dioxide layer 24 which covered the upper face of the blank.
  • directional reactive ion etching directional ion etching (directional RIE) was used so as to remove silicon dioxide only on the upper face.
  • the following figure illustrates the SOI wafer 22 after the deposition of a layer of photosensitive resin 28 completely covering the blank.
  • the resin can be, for example, of the AZ® 1518 type. It can be applied with a spinner at a speed of 4000 revolutions / minute so that the thickness of the layer 28 is about 2.6 microns.
  • the figure 22 illustrates the SOI wafer 22 after the production of an openwork mask by structuring the resin layer 28.
  • the structuring of the layer 28 is carried out by photolithography by implementing the RIE etching. It will be understood that the apertures of the mask are arranged so as to expose only the surfaces to be roughened.
  • the figure 22 also shows a sacrificial layer 30 which was then deposited on the resin layer 28 and in the openings of the latter.
  • the sacrificial layer 30 can for example be produced by applying photosensitive resin of the AZ® 1518 type with a spinner at 5000 revolutions / minute.
  • the figure 23 illustrates the SOI wafer 22, as well as the timepiece component blank which is formed in the upper layer of the latter, after the transfer by DRIE etching of inhomogeneities of the sacrificial layer 30 on the places to be roughened of the blank.
  • the figure 23 further shows that the resin residues of the perforated mask 28 and of the sacrificial layer 30, as well as the residues of C4F8 left by the passivation steps have been removed.
  • the figure 23 finally shows that the SiO 2 which covered the side faces of the blank has also been eliminated.
  • the horological component blank can finally be detached from the remainder of the SOI wafer 22.
  • the SOI wafer and the blank are immersed in a bath which contains a chemical agent which attacks the silicon dioxide while sparing the silicon.
  • a chemical agent which attacks the silicon dioxide while sparing the silicon Preferably, buffered hydrofluoric acid (BHF) is used.

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  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Micromachines (AREA)
  • Weting (AREA)
EP19185364.7A 2019-07-10 2019-07-10 Verfahren zum abschnittsweisen satinieren einer uhrenkomponente aus silizium Active EP3764169B1 (de)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4700499A2 (de) 2019-07-10 2026-02-25 Patek Philippe Sa Geneve Verfahren zur herstellung einer uhrkomponente, deren oberfläche zumindest teilweise mit einer farbschicht beschichtet ist

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4206826B1 (de) * 2021-12-30 2026-04-29 Rubattel et Weyermann S.A. Verfahren zur herstellung von appliken auf einem zifferblatt
CH721146A1 (fr) * 2023-09-21 2025-03-31 Richemont Int Sa Procédé de fabrication de composants horlogers en silicium

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994014187A1 (de) 1992-12-05 1994-06-23 Robert Bosch Gmbh Verfahren zum anisotropen ätzen von silicium
FR2901635A1 (fr) * 2006-06-09 2007-11-30 Commissariat Energie Atomique Dispositif de connexion tridimensionnel dans un substrat
EP2856903A1 (de) * 2013-10-01 2015-04-08 Montres Rado S.A. Keramikelement mit mindestens einem Keramikdekoreinsatz
CH708827A2 (fr) * 2013-11-08 2015-05-15 Nivarox Sa Pièce de micromécanique creuse, à plusieurs niveaux fonctionnels et monobloc en un matériau à base d'un allotrope synthétique du carbone.
EP3002635A1 (de) * 2014-09-29 2016-04-06 Richemont International S.A. Herstellungsverfahren eines federelements für uhrwerk oder anderes präzisionsinstrument
EP3109199A1 (de) * 2015-06-25 2016-12-28 Nivarox-FAR S.A. Werkstück auf siliziumbasis mit mindestens einer fase, und sein herstellungsverfahren
EP3192645A1 (de) * 2016-01-12 2017-07-19 Commissariat À L'Énergie Atomique Et Aux Énergies Alternatives Herstellungsverfahren eines bildschirms, der mit rückstrahlenden mikrostrukturen ausgestattet ist

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994014187A1 (de) 1992-12-05 1994-06-23 Robert Bosch Gmbh Verfahren zum anisotropen ätzen von silicium
FR2901635A1 (fr) * 2006-06-09 2007-11-30 Commissariat Energie Atomique Dispositif de connexion tridimensionnel dans un substrat
EP2856903A1 (de) * 2013-10-01 2015-04-08 Montres Rado S.A. Keramikelement mit mindestens einem Keramikdekoreinsatz
CH708827A2 (fr) * 2013-11-08 2015-05-15 Nivarox Sa Pièce de micromécanique creuse, à plusieurs niveaux fonctionnels et monobloc en un matériau à base d'un allotrope synthétique du carbone.
EP3002635A1 (de) * 2014-09-29 2016-04-06 Richemont International S.A. Herstellungsverfahren eines federelements für uhrwerk oder anderes präzisionsinstrument
EP3109199A1 (de) * 2015-06-25 2016-12-28 Nivarox-FAR S.A. Werkstück auf siliziumbasis mit mindestens einer fase, und sein herstellungsverfahren
EP3192645A1 (de) * 2016-01-12 2017-07-19 Commissariat À L'Énergie Atomique Et Aux Énergies Alternatives Herstellungsverfahren eines bildschirms, der mit rückstrahlenden mikrostrukturen ausgestattet ist

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP4700499A2 (de) 2019-07-10 2026-02-25 Patek Philippe Sa Geneve Verfahren zur herstellung einer uhrkomponente, deren oberfläche zumindest teilweise mit einer farbschicht beschichtet ist

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