WO2023042834A1 - Method for producing crystal device - Google Patents

Method for producing crystal device Download PDF

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Publication number
WO2023042834A1
WO2023042834A1 PCT/JP2022/034326 JP2022034326W WO2023042834A1 WO 2023042834 A1 WO2023042834 A1 WO 2023042834A1 JP 2022034326 W JP2022034326 W JP 2022034326W WO 2023042834 A1 WO2023042834 A1 WO 2023042834A1
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gold
layer
metal
silver
crystal device
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PCT/JP2022/034326
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French (fr)
Japanese (ja)
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公彦 竹内
裕 矢部
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株式会社ジェナジー
株式会社昭和真空
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Priority to JP2022555910A priority Critical patent/JP7433592B2/en
Priority to CN202280062672.8A priority patent/CN117941252A/en
Publication of WO2023042834A1 publication Critical patent/WO2023042834A1/en

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    • H—ELECTRICITY
    • H03—ELECTRONIC CIRCUITRY
    • H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
    • H03H3/00—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators
    • H03H3/007—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks
    • H03H3/02—Apparatus or processes specially adapted for the manufacture of impedance networks, resonating circuits, resonators for the manufacture of electromechanical resonators or networks for the manufacture of piezoelectric or electrostrictive resonators or networks
    • H—ELECTRICITY
    • H03—ELECTRONIC CIRCUITRY
    • H03H—IMPEDANCE NETWORKS, e.g. RESONANT CIRCUITS; RESONATORS
    • H03H9/00—Networks comprising electromechanical or electro-acoustic devices; Electromechanical resonators
    • H03H9/15—Constructional features of resonators consisting of piezoelectric or electrostrictive material
    • H03H9/17—Constructional features of resonators consisting of piezoelectric or electrostrictive material having a single resonator
    • H03H9/19—Constructional features of resonators consisting of piezoelectric or electrostrictive material having a single resonator consisting of quartz

Definitions

  • the present invention relates to a method for manufacturing a crystal device.
  • Crystal devices are used in a wide variety of electronic devices such as digital cameras, smartphones, watches, personal computers, televisions, and media players.
  • a crystal device is a component that produces a reference signal (clock) that is indispensable for digital control, and is an important component that acts as the heart of a human being. (Patent Document 1).
  • a technique of using a gold-silver alloy for example, 22-karat gold or 20-karat gold, etc.
  • the process of recovering and refining gold or the like adhering to the target material used in the main sputtering apparatus is more complicated than in the case of a single metal, and the cost reduction effect is small.
  • the object of the present invention is to provide a crystal device that enables cost reduction of noble metal targets as raw material costs without deteriorating aging characteristics.
  • the method for manufacturing a crystal device of the present invention comprises a base layer, a layer containing gold and a second metal, a layer containing gold and a second metal, and a layer containing gold and gold in this order from the surface of the crystal resonator element using a carousel sputtering apparatus. , a layer comprising a second metal and having at least 50% by volume of the second metal, gold, a layer comprising the second metal and having less than 50% by volume of the second metal, and 95% by volume of gold % or more of the metal.
  • the second metal may be a silver layer.
  • FIG. 1 is a plan view (viewed from above) of a carousel-type three-source sputtering apparatus used in the method of manufacturing a crystal device according to the present embodiment, and is a view showing a film forming chamber.
  • FIG. FIG. 1 is a schematic vertical cross-sectional view of electrodes of a crystal device deposited in this embodiment, and one circle is the size of a molecule such as gold.
  • FIG. 1 is a schematic vertical cross-sectional view of electrodes of a crystal device deposited in this embodiment, and one circle is the size of a molecule such as gold.
  • FIG. 1 is a schematic vertical cross-sectional view of electrodes of a crystal device formed in a modified embodiment, and one circle is the size of a molecule such as gold. In FIG. is arranged, but it is omitted on one side.
  • FIG. 1A is a plan view of the crystal vibrating piece 12
  • FIG. 1B is a front view of the crystal vibrating piece 12
  • FIG. 1C is a bottom view of the crystal vibrating piece 12.
  • the electrode 3A in FIG. 1A is arranged so that the electrode 3A largely occupies the plane of the crystal vibrating piece 12 .
  • the electrode 3B is arranged so as to occupy the lower right end of the plane of the crystal vibrating piece 12 in a small area.
  • electrodes 3A and 3B are arranged so as to continue from FIG. 1(A).
  • the electrode 3B is arranged so that the bottom surface of the crystal vibrating piece 12 is largely occupied as continued from FIG. 1(B).
  • the method for manufacturing the crystal device 1 of the present embodiment uses the carousel type three-source sputtering apparatus 10 shown in FIG.
  • the carousel type three-source sputtering apparatus 10 revolves and rotates a substrate 13 on which several tens to several hundreds of crystal vibrating pieces (workpieces) 12 are set. 18 are placed and sputtering is performed to continuously form films of dissimilar metals.
  • the carousel type three-source sputtering apparatus 10 has a revolution speed of 5 to 99 rpm, rotates in the direction of the arrow M, has a short idle movement time, and has individual sputtering targets 14, 16, 18 (chromium target 14, An arbitrary film composition can be formed by controlling the film forming power of the silver target 16 and the gold target 18) or ON/OFF of the power supply.
  • the power to the silver target 16 and gold target 18 is turned off.
  • the film forming power is reduced and/or the film forming time is shortened.
  • a chromium layer as a base layer is formed on the surface of the crystal vibrating piece 12
  • a gold film is formed on the surface of the base layer, and then silver and gold are alternately laminated.
  • a gold film is deposited on the surface layer furthest from the underlying layer.
  • FIG. 3 shows the layered structure of each film in this way.
  • a layer 30 having chromium 20, gold 22, and silver 24, which are constituent elements of the underlying layer is formed in order from the surface of the crystal resonator element (workpiece 12).
  • a layer 32 containing gold 22 and silver 24 and containing 50% by volume or more of silver 24 is formed.
  • a layer 34 comprising gold 22 and silver 24 with less than 50% by volume of silver 24 is then deposited.
  • a layer 36 containing 95% by volume or more of gold 22 is deposited.
  • the crystal device 1 is now manufactured.
  • the crystal device 1 that enables cost reduction of the noble metal target without degrading the aging characteristics. It is said that the aging characteristics of the electrodes of the crystal device 1 do not deteriorate because the gold electrodes contain less easily oxidizable materials (silver, iron, chromium, etc.). In this respect, according to the present embodiment, since silver and gold are alternately laminated, the gold electrode contains less materials that are easily oxidized, and the aging characteristics are not degraded.
  • a gold/silver alloy target has been put into practical use for forming the electrodes of the crystal device 1 .
  • this alloy target can reduce the cost by reducing the weight of gold, it is necessary to form a uniform alloy composition, and to recover precious metals such as defective products or anti-adhesion plates, gold 22 and silver 24 are used. Refining is required, man-hours are required, and the cost reduction rate is inferior to others. In this respect as well, the method of forming the electrodes of the crystal device 1 of the present embodiment is superior.
  • the concentration of silver 24 can be gradually changed (layers 32, 34, and 36). , the volume change due to the temperature of each layer can be moderated, and film stress and the like can be suppressed.
  • the film formation speed of the carousel type three-source sputtering apparatus 10 is almost the same as the film formation speed of the so-called inter-back type sputtering.
  • film formation can be performed at a rate several times to several tens of times higher than that of the so-called inter-back type sputtering.
  • inter-back type sputtering compared to the carousel type multi-source sputtering apparatus 10, idle movement time is increased and the productivity (apparatus capacity) of the sputtering process is deteriorated.
  • one or two substrates 13 on which several tens to several hundreds of crystal vibrating pieces 12 are set are placed on a conveying jig, and are spaced between the targets. is moved back and forth, but the film formation is only the forward trip, and the return trip is an idle movement. make worse.
  • the film can be formed by rotating 8 to 12 substrates 13 in a fixed direction. Since the time does not change, the productivity (apparatus capacity) of the sputtering process is not deteriorated.
  • the silver 24 and the like are slightly exposed in the cross section in the film thickness direction during the layered film formation of the silver 24, the gold 22 and the like. However, this degree of exposure hardly degrades the aging characteristics of the crystal device 1 .
  • silver 24 and gold 22 are deposited in a layered manner, but instead of silver 24 (second metal), one, two, or three layers of titanium, tungsten, nickel, or the like are used. Seeds may be used.
  • the carousel-type three-source sputtering apparatus 10 is used in the present embodiment, but a carousel-type four-source sputtering apparatus or the like may be used to use sputtering targets of other elements or multiple elements. .
  • the carousel sputtering apparatus 10 is used to sequentially form a base layer, a layer containing gold and a second metal, a layer containing gold and a second metal, and a layer containing gold and a second metal.
  • a layer containing 50% by volume or more of the second metal, a layer containing gold and a second metal and containing less than 50% by volume of the second metal, and a layer formed of a metal containing 95% by volume or more of gold. is deposited.
  • FIG. 4 shows a layered structure of each film of a crystal device 40 which is a modification of the crystal device 1 .
  • a layer 64 containing chromium 60, gold 62, and silver 66, which are constituent elements of the underlying layer is deposited in order from the surface of the plate-shaped crystal 42.
  • a layer 68 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited.
  • a layer 70 having gold 62 and silver 66 with silver 24 sparse is then deposited.
  • a layer 72 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited.
  • a layer 74 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited.
  • a layer 76 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited.
  • a layer 78 is then deposited having gold 62 and silver 66 with less than 50% silver 66 by volume.
  • a layer 80 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited.
  • a layer 82 having gold 62 and 95% by volume or more is then deposited. The crystal device 40 is now manufactured.
  • the crystal device 40 that enables a reduction in the cost of precious metals as raw materials without degrading the aging characteristics, like the crystal device 1 .
  • the electrodes of the crystal device 40 do not degrade the aging characteristics if the gold electrodes do not contain a material that is easily oxidized (silver, iron, chromium, etc.).
  • the gold electrode contains less material that is easily oxidized, and the aging characteristics are improved, as in the crystal device 1. do not lower.
  • Reference Signs List 1 40 crystal device 10 carousel sputtering device 12 crystal vibrating piece (workpiece) 22,62 gold 24,66 second metal (silver) 30, 64 Underlayer 32, 34, 36, 68, 70, 72, 74, 76, 78, 80, 82 Layer

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Physics & Mathematics (AREA)
  • Acoustics & Sound (AREA)
  • Physical Vapour Deposition (AREA)
  • Piezo-Electric Or Mechanical Vibrators, Or Delay Or Filter Circuits (AREA)

Abstract

[Problem] To provide a crystal device which makes it possible to reduce the cost for noble metal as a material cost without decreasing aging characteristics.　[Solution] The present invention uses a carousel-type sputtering device 10 to form a film that has, in the following order from the surface of a crystal resonator piece, an underlayer, a layer that has gold and a second metal, a layer that has gold and the second metal and has the second metal in an amount of 50 vol% or more, a layer that has gold and the second metal and has the second metal in an amount of less than 50 vol%, and a layer that is formed from a metal having 95 vol% or more of gold.

Description

水晶デバイスの製造法Crystal device manufacturing method
　本発明は、水晶デバイスの製造法に関する。 The present invention relates to a method for manufacturing a crystal device.
　水晶デバイスは、デジタルカメラ、スマートフォン、時計、パーソナルコンピュータ、テレビ、メディアプレーヤ等の多岐にわたる電子機器等に用いられている。水晶デバイスは、デジタル制御には欠かせない基準信号（クロック）を作り出す部品で、人間にたとえると「心臓」のやくわりをする重要な部品である。（特許文献１）。 Crystal devices are used in a wide variety of electronic devices such as digital cameras, smartphones, watches, personal computers, televisions, and media players. A crystal device is a component that produces a reference signal (clock) that is indispensable for digital control, and is an important component that acts as the heart of a human being. (Patent Document 1).
特開２０１３－０８９９９４号公報JP 2013-089994 A
　周波数経時変化（エージング特性）が重要な特性になってきた中で、水晶振動片の電極は、銀電極から金電極が主流になってきている。しかしながら金は、材料代が高価であり、水晶デバイスのコストアップの要因となっていた。 As the change in frequency over time (aging characteristics) has become an important characteristic, the electrodes of crystal vibrating pieces are shifting from silver electrodes to gold electrodes. However, gold is expensive as a material and has been a factor in increasing the cost of crystal devices.
　一つの改善策として、電極材料を金銀合金（たとえば、２２金または２０金等）にする技術も実用化されている。しかしながら、主力のスパッタリング装置で使用するターゲット材の装置等に付着した金等を回収し、精製する工程が、単一金属の場合に比べ、複雑であり、コストダウン効果が少ない。 As one improvement measure, a technique of using a gold-silver alloy (for example, 22-karat gold or 20-karat gold, etc.) as the electrode material has also been put into practical use. However, the process of recovering and refining gold or the like adhering to the target material used in the main sputtering apparatus is more complicated than in the case of a single metal, and the cost reduction effect is small.
　また、金銀合金ターゲットを用いて成膜した場合は、銀が金の中にまんべんなく分布するため、電極最表面にも銀成分が分布する。このため、水晶デバイスのパッケージ内に残留するアウトガスと反応して、金電極品と比較すると、エージング特性が悪化する原因となっている。 In addition, when a gold-silver alloy target is used to form a film, silver is evenly distributed in the gold, so the silver component is also distributed on the outermost surface of the electrode. For this reason, it reacts with the outgas remaining in the package of the crystal device, causing the deterioration of the aging characteristics as compared with the gold electrode product.
　そこで本発明の目的は、エージング特性を低下させずに、原材料費としての貴金属ターゲットのコストダウンを可能にする水晶デバイスを提供することである。 Therefore, the object of the present invention is to provide a crystal device that enables cost reduction of noble metal targets as raw material costs without deteriorating aging characteristics.
　上記目的を達成するため、本発明の水晶デバイスの製造法は、カルーセル式スパッタリング装置を用いて、水晶振動片の表面から順に、下地層と金と第２の金属とを有する層と、金と、第２の金属を有し、第２の金属を５０体積％以上有する層と、金と、第２の金属を有し、第２の金属を５０体積％未満有する層と、金を９５体積％以上有する金属で成膜する層と、を有するように成膜する。 In order to achieve the above object, the method for manufacturing a crystal device of the present invention comprises a base layer, a layer containing gold and a second metal, a layer containing gold and a second metal, and a layer containing gold and gold in this order from the surface of the crystal resonator element using a carousel sputtering apparatus. , a layer comprising a second metal and having at least 50% by volume of the second metal, gold, a layer comprising the second metal and having less than 50% by volume of the second metal, and 95% by volume of gold % or more of the metal.
　ここで、第２の金属は、銀層である、こととしても良い。 Here, the second metal may be a silver layer.
　本発明ではエージング特性を低下させずに、原材料費としての貴金属のコストダウンを可能にする水晶デバイスを提供することができる。 With the present invention, it is possible to provide a crystal device that enables a reduction in the cost of precious metals as raw materials without deteriorating aging characteristics.
水晶振動片と、電極の配置を示し、（Ａ）は水晶振動片の平面図であり、（Ｂ）は水晶振動片の正面図であり、（Ｃ）は水晶振動片の底面図である。The crystal vibrating piece and the arrangement of the electrodes are shown, (A) is a plan view of the crystal vibrating piece, (B) is a front view of the crystal vibrating piece, and (C) is a bottom view of the crystal vibrating piece. 本実施の形態の水晶デバイスの製造法に用いる、カルーセル式３源スパッタリング装置の平面図（上から見た図）であり、成膜室を示す図である。1 is a plan view (viewed from above) of a carousel-type three-source sputtering apparatus used in the method of manufacturing a crystal device according to the present embodiment, and is a view showing a film forming chamber. FIG. 本実施の形態で成膜した、水晶デバイスの電極の縦断面模式図であり、一つの丸が金等の分子の大きさのものである、図１では、水晶振動片の両面に電極が配置されるが、それを片面だけに省略した図である。FIG. 1 is a schematic vertical cross-sectional view of electrodes of a crystal device deposited in this embodiment, and one circle is the size of a molecule such as gold. In FIG. 1, electrodes are arranged on both sides of the crystal vibrating piece However, it is a diagram that omits it only on one side. 変形例の実施の形態で成膜した、水晶デバイスの電極の縦断面模式図であり、一つの丸が金等の分子の大きさのものである、図１では、水晶振動片の両面に電極が配置されるが、それを片面だけに省略した図である。FIG. 1 is a schematic vertical cross-sectional view of electrodes of a crystal device formed in a modified embodiment, and one circle is the size of a molecule such as gold. In FIG. is arranged, but it is omitted on one side.
（本実施の形態の水晶デバイスの製造法）
　以下、本の形態の水晶デバイスの製造法について、図１と図２に基づいて説明する。本実施の形態で用いる水晶デバイス１は、図１に示すような水晶振動片１２と、電極３Ａ，３Ｂの配置となっている。図１の（Ａ）は水晶振動片１２の平面図であり、図１の（Ｂ）は水晶振動片１２の正面図であり、図１の（Ｃ）は水晶振動片１２の底面図である。 (Manufacturing method of the crystal device of the present embodiment)
A method of manufacturing a crystal device in the form of a book will be described below with reference to FIGS. 1 and 2. FIG. The crystal device 1 used in this embodiment has a crystal vibrating piece 12 and electrodes 3A and 3B arranged as shown in FIG. 1A is a plan view of the crystal vibrating piece 12, FIG. 1B is a front view of the crystal vibrating piece 12, and FIG. 1C is a bottom view of the crystal vibrating piece 12. .
　図１（Ａ）の、電極３Ａは、水晶振動片１２の平面を電極３Ａが大きく占めるように配置されている。電極３Ｂは、水晶振動片１２の平面の右下端を小さく占めるように配置されている。図１（Ｂ）は、図１（Ａ）から続くように電極３Ａ，３Ｂが配置されている。図１（Ｃ）は、図１（Ｂ）から続くように水晶振動片１２の底面を電極３Ｂが大きく占めるように配置されている。 The electrode 3A in FIG. 1A is arranged so that the electrode 3A largely occupies the plane of the crystal vibrating piece 12 . The electrode 3B is arranged so as to occupy the lower right end of the plane of the crystal vibrating piece 12 in a small area. In FIG. 1(B), electrodes 3A and 3B are arranged so as to continue from FIG. 1(A). In FIG. 1(C), the electrode 3B is arranged so that the bottom surface of the crystal vibrating piece 12 is largely occupied as continued from FIG. 1(B).
　本実施の形態の水晶デバイス１の製造法は、図２に示すカルーセル式３源スパッタリング装置１０を用いる。カルーセル式３源スパッタリング装置１０とは、水晶振動片（ワーク）１２が数十～数百個セットされた基板１３を公転回転させ、ワーク１２に対向する３ヶ所の位置にスパッタリングターゲット１４，１６，１８を配置し、スパッタリングを行うことで、連続的に異種金属を成膜できる装置である。 The method for manufacturing the crystal device 1 of the present embodiment uses the carousel type three-source sputtering apparatus 10 shown in FIG. The carousel type three-source sputtering apparatus 10 revolves and rotates a substrate 13 on which several tens to several hundreds of crystal vibrating pieces (workpieces) 12 are set. 18 are placed and sputtering is performed to continuously form films of dissimilar metals.
　このカルーセル式３源スパッタリング装置１０の公転回転速度は、５～９９ｒｐｍであり、矢印Ｍの方向に回転し、空移動時間が少なく、また、個々のスパッタリングターゲット１４，１６，１８（クロムターゲット１４、銀ターゲット１６、金ターゲット１８）の成膜パワーまたは、電源のＯＮ／ＯＦＦを制御することで、任意の膜組成を形成できる。 The carousel type three-source sputtering apparatus 10 has a revolution speed of 5 to 99 rpm, rotates in the direction of the arrow M, has a short idle movement time, and has individual sputtering targets 14, 16, 18 (chromium target 14, An arbitrary film composition can be formed by controlling the film forming power of the silver target 16 and the gold target 18) or ON/OFF of the power supply.
　たとえば、下地層であるクロムターゲット１４を最初に成膜するときは、銀ターゲット１６、金ターゲット１８の電源をＯＦＦにする。また、銀またはクロムの薄い成膜をするときは、成膜パワーを小さくする、および／または成膜時間を短くする。金の厚い成膜をするときは、成膜パワーを大きくする、および／または成膜時間を長くする。 For example, when the chromium target 14, which is the underlying layer, is deposited first, the power to the silver target 16 and gold target 18 is turned off. Also, when forming a thin film of silver or chromium, the film forming power is reduced and/or the film forming time is shortened. When depositing a thick gold film, increase the deposition power and/or lengthen the deposition time.
　そして、カルーセル式３源スパッタリング装置１０を用いて、水晶振動片１２の表面に下地層であるクロム層を成膜し、下地層の表面に金を成膜し、その後銀と金を交互に積層成膜し、下地層から一番遠い表面層に金を成膜する。 Then, using the carousel-type three-source sputtering apparatus 10, a chromium layer as a base layer is formed on the surface of the crystal vibrating piece 12, a gold film is formed on the surface of the base layer, and then silver and gold are alternately laminated. A gold film is deposited on the surface layer furthest from the underlying layer.
　このように、各成膜を積層したものを図３に示す。まず、カルーセル式３源スパッタリング装置１０を用いて、水晶振動片（ワーク１２）の表面から順に、下地層の構成要素であるクロム２０と、金２２と、銀２４を有する層３０を成膜する。次いで、金２２と、銀２４を有し、銀２４を５０体積％以上にした層３２を成膜する。次いで、金２２と、銀２４を有し、銀２４を５０体積％未満にした層３４を成膜する。次いで、金２２を９５体積％以上有する層３６を成膜する。これで、水晶デバイス１が製造される。 FIG. 3 shows the layered structure of each film in this way. First, using the carousel-type three-source sputtering apparatus 10, a layer 30 having chromium 20, gold 22, and silver 24, which are constituent elements of the underlying layer, is formed in order from the surface of the crystal resonator element (workpiece 12). . Next, a layer 32 containing gold 22 and silver 24 and containing 50% by volume or more of silver 24 is formed. A layer 34 comprising gold 22 and silver 24 with less than 50% by volume of silver 24 is then deposited. Next, a layer 36 containing 95% by volume or more of gold 22 is deposited. The crystal device 1 is now manufactured.
　（本実施の形態によって得られる主な効果）
　本実施の形態によれば、エージング特性を低下させずに、貴金属ターゲットのコストダウンを可能にする水晶デバイス１を提供することができる。水晶デバイス１の電極は、金電極が、酸化しやすい材料（銀、鉄、クロム等）の含有が少ないこと等が、エージング特性を低下させないと言われている。その点、本実施の形態によれば、銀と金を交互に積層成膜していることから、金電極、が酸化しやすい材料の含有が少なく、エージング特性を低下させない。 (Main effects obtained by this embodiment)
According to this embodiment, it is possible to provide the crystal device 1 that enables cost reduction of the noble metal target without degrading the aging characteristics. It is said that the aging characteristics of the electrodes of the crystal device 1 do not deteriorate because the gold electrodes contain less easily oxidizable materials (silver, iron, chromium, etc.). In this respect, according to the present embodiment, since silver and gold are alternately laminated, the gold electrode contains less materials that are easily oxidized, and the aging characteristics are not degraded.
　また、水晶デバイス１の電極を形成するのに、金／銀合金ターゲットが実用化されている。しかし、この合金ターゲットは、金重量が減る分のコストダウンは可能になるが、均一な合金組成に形成すること、故品または防着板等の貴金属を回収するのに金２２と銀２４の精製が必要であり、工数がかかり、コストダウン率は以外に劣る。この点でも本実施の形態の水晶デバイス１の電極を形成方法は、優位性がある。 Also, a gold/silver alloy target has been put into practical use for forming the electrodes of the crystal device 1 . However, although this alloy target can reduce the cost by reducing the weight of gold, it is necessary to form a uniform alloy composition, and to recover precious metals such as defective products or anti-adhesion plates, gold 22 and silver 24 are used. Refining is required, man-hours are required, and the cost reduction rate is inferior to others. In this respect as well, the method of forming the electrodes of the crystal device 1 of the present embodiment is superior.
　また、層３０、層３２，層３４，層３６をこの順に水晶振動片１２の表面から積層することで、特に銀２４の濃度を少しずつ変えることができ（層３２，層３４，層３６）、各層の温度による体積変化を緩やかにし、膜応力等を抑制できる。 In addition, by stacking the layers 30, 32, 34, and 36 in this order from the surface of the crystal vibrating piece 12, the concentration of silver 24 can be gradually changed ( layers 32, 34, and 36). , the volume change due to the temperature of each layer can be moderated, and film stress and the like can be suppressed.
　また、本来、カルーセル式３源スパッタリング装置１０の成膜速度は、いわゆるインターバック式のスパッタリングの成膜速度とほとんど変わらない。しかし、カルーセル式の多源スパッタリング装置１０を用いると、いわゆるインターバック式のスパッタリングに比べ、たとえば数倍～数十倍の速度で成膜できる。いわゆるインターバック式のスパッタリングは、カルーセル式の多源スパッタリング装置１０に比べ、空移動時間が増えてスパッタリング工程の生産性（装置能力）を悪化させる。 In addition, originally, the film formation speed of the carousel type three-source sputtering apparatus 10 is almost the same as the film formation speed of the so-called inter-back type sputtering. However, by using the carousel type multi-source sputtering apparatus 10, film formation can be performed at a rate several times to several tens of times higher than that of the so-called inter-back type sputtering. In the so-called inter-back type sputtering, compared to the carousel type multi-source sputtering apparatus 10, idle movement time is increased and the productivity (apparatus capacity) of the sputtering process is deteriorated.
　言い換えると、いわゆるインターバック式のスパッタリング装置で本発明の積層成膜をする場合、水晶振動片１２が数十～数百個セットされた基板１３を１～２枚搬送治具に載せてターゲット間を往復移動させるが成膜は往路のみであり復路は、空移動になるため多源になればなるほど、また、積層が多くなるほどから空移動時間が増えてスパッタリング工程の生産性（装置能力）を悪化させる。 In other words, when the multilayer film formation of the present invention is performed using a so-called inter-back type sputtering apparatus, one or two substrates 13 on which several tens to several hundreds of crystal vibrating pieces 12 are set are placed on a conveying jig, and are spaced between the targets. is moved back and forth, but the film formation is only the forward trip, and the return trip is an idle movement. make worse.
　しかし、カルーセル式スパッタリング装置１０を用いると、基板１３をたとえば８～１２枚一定方向に回転させることで成膜できるため、ターゲットの種類がたとえば２源から３源、あるいは４源と増えても回転時間は変わらないためスパッタリング工程の生産性(装置能力)を悪化させることはない。 However, when the carousel type sputtering apparatus 10 is used, the film can be formed by rotating 8 to 12 substrates 13 in a fixed direction. Since the time does not change, the productivity (apparatus capacity) of the sputtering process is not deteriorated.
　なお、銀２４、金２２等の積層成膜の際に、膜厚方向の断面に銀２４等が若干露出する。しかし、この程度の露出は、水晶デバイス１のエージング特性を殆ど低下させない。 It should be noted that the silver 24 and the like are slightly exposed in the cross section in the film thickness direction during the layered film formation of the silver 24, the gold 22 and the like. However, this degree of exposure hardly degrades the aging characteristics of the crystal device 1 .
　（他の形態）
　上述した本実施の形態に係る水晶デバイス１の製造法は、本発明の好適な形態の一例ではあるが、これに限定されるものではなく本発明の要旨を変更しない範囲において種々の変形実施が可能である。 (other forms)
The method of manufacturing the crystal device 1 according to the present embodiment described above is an example of a preferred embodiment of the present invention, but it is not limited to this, and various modifications can be made without changing the gist of the present invention. It is possible.
　たとえば、本実施の形態では、銀２４と金２２を積層成膜する等しているが、この銀２４（第２の金属）に代えてチタン層、タングステン層、ニッケル等の１または２または３種を用いてもよい。 For example, in the present embodiment, silver 24 and gold 22 are deposited in a layered manner, but instead of silver 24 (second metal), one, two, or three layers of titanium, tungsten, nickel, or the like are used. Seeds may be used.
　また、そのためには、本実施の形態では、カルーセル式３源スパッタリング装置１０を用いているが、カルーセル式４源スパッタリング装置等を用いて、他元素・多元素のスパッタリングターゲットを用いることとしても良い。 For this purpose, the carousel-type three-source sputtering apparatus 10 is used in the present embodiment, but a carousel-type four-source sputtering apparatus or the like may be used to use sputtering targets of other elements or multiple elements. .
　本実施の形態では、カルーセル式スパッタリング装置１０を用いて、水晶振動片の表面から順に、下地層と金と第２の金属とを有する層と、金と、第２の金属を有し、第２の金属を５０体積％以上有する層と、金と、第２の金属を有し、第２の金属を５０体積％未満有する層と、金を９５体積％以上有する金属で成膜する層と、を有するように成膜する。 In this embodiment, the carousel sputtering apparatus 10 is used to sequentially form a base layer, a layer containing gold and a second metal, a layer containing gold and a second metal, and a layer containing gold and a second metal. A layer containing 50% by volume or more of the second metal, a layer containing gold and a second metal and containing less than 50% by volume of the second metal, and a layer formed of a metal containing 95% by volume or more of gold. , is deposited.
（水晶デバイス１の変形例）
　そして、水晶デバイス１の変形例の水晶デバイス４０の各成膜を積層したものを図４に示す。まず、カルーセル式３源スパッタリング装置１０を用いて、板状の水晶４２の表面から順に、下地層の構成要素であるクロム６０と、金６２と、銀６６を有する層６４を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層６８を成膜する。次いで、金６２と、銀６６を有し、銀２４を疎にした層７０を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層７２を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層７４を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層７６を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層７８を成膜する。次いで、金６２と、銀６６を有し、銀６６を５０体積％未満にした層８０を成膜する。次いで、金６２と、９５体積％以上を有する層８２を成膜する。これで、水晶デバイス４０が製造される。 (Modified example of crystal device 1)
FIG. 4 shows a layered structure of each film of a crystal device 40 which is a modification of the crystal device 1 . First, using the carousel three-source sputtering apparatus 10, a layer 64 containing chromium 60, gold 62, and silver 66, which are constituent elements of the underlying layer, is deposited in order from the surface of the plate-shaped crystal 42. As shown in FIG. A layer 68 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited. A layer 70 having gold 62 and silver 66 with silver 24 sparse is then deposited. A layer 72 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited. A layer 74 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited. A layer 76 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited. A layer 78 is then deposited having gold 62 and silver 66 with less than 50% silver 66 by volume. A layer 80 comprising gold 62 and silver 66 with less than 50 volume percent silver 66 is then deposited. A layer 82 having gold 62 and 95% by volume or more is then deposited. The crystal device 40 is now manufactured.
　（変形例の実施の形態によって得られる主な効果）
　変形例の形態によれば、エージング特性を低下させずに、原材料費としての貴金属のコストダウンを可能にする水晶デバイス４０を、水晶デバイス１と同様に提供することができる。水晶デバイス４０の電極は、金電極が酸化しやすい材料（銀、鉄、クロム等）の含有が少ないこと等が、エージング特性を低下させないと言われているのは、水晶デバイス１と同様である。その点、変形例の実施の形態によれば、銀と金を交互に積層成膜していることから、水晶デバイス１と同様に、金電極が酸化しやすい材料の含有が少なく、エージング特性を低下させない。 (Main Effects Obtained by Modified Embodiment)
According to the form of the modification, it is possible to provide the crystal device 40 that enables a reduction in the cost of precious metals as raw materials without degrading the aging characteristics, like the crystal device 1 . As with the crystal device 1, it is said that the electrodes of the crystal device 40 do not degrade the aging characteristics if the gold electrodes do not contain a material that is easily oxidized (silver, iron, chromium, etc.). . In this respect, according to the embodiment of the modified example, since silver and gold are alternately laminated, the gold electrode contains less material that is easily oxidized, and the aging characteristics are improved, as in the crystal device 1. do not lower.
　１，４０　水晶デバイス
　１０　カルーセル式スパッタリング装置
　１２　水晶振動片（ワーク）
　２２，６２　金
　２４，６６　第２の金属（銀）
　３０，６４　下地層
　３２，３４，３６，６８，７０，７２，７４，７６，７８，８０，８２　層

  Reference Signs List 1, 40 crystal device 10 carousel sputtering device 12 crystal vibrating piece (workpiece)
22,62 gold 24,66 second metal (silver)
30, 64 Underlayer 32, 34, 36, 68, 70, 72, 74, 76, 78, 80, 82 Layer

Claims (2)

  1. 　カルーセル式スパッタリング装置を用いて、
    　水晶振動片の表面から順に、下地層と金と第２の金属とを有する層と、
    　前記金と、前記第２の金属を有し、前記第２の金属を５０体積％以上有する層と、
    　前記金と、前記第２の金属を有し、前記第２の金属を５０体積％未満有する層と、
    　前記金を９５体積％以上有する金属で成膜する層と、を有するように成膜する、
    　水晶デバイスの製造法。     Using a carousel type sputtering device,
    a layer having an underlying layer, gold, and a second metal in order from the surface of the crystal vibrating piece;
    a layer containing the gold and the second metal and containing 50% by volume or more of the second metal;
    a layer comprising the gold and the second metal, the layer comprising less than 50% by volume of the second metal;
    and a layer formed of a metal having 95% by volume or more of the gold,
    Manufacturing method of quartz device.
  2. 　請求項１記載の水晶デバイスの製造法であって、
    　前記第２の金属は、銀層である、
    　水晶デバイスの製造法。
          A method for manufacturing a crystal device according to claim 1,
    wherein the second metal is a silver layer;
    Manufacturing method of quartz device.
PCT/JP2022/034326 2021-09-19 2022-09-14 Method for producing crystal device WO2023042834A1 (en)

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Citations (4)

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JPS5637522U (en) * 1979-08-28 1981-04-09
JP2005136575A (en) * 2003-10-29 2005-05-26 Seiko Epson Corp Piezoelectric vibrating piece, structure of excitation electrode thereof, electrode forming method, piezoelectric device, cellular telephone device employing piezoelectric device and electronic equipment employing piezoelectric device
WO2015004755A1 (en) * 2013-07-10 2015-01-15 株式会社シンクロン Optical film thickness measurement device, thin film forming device, and method for measuring film thickness
JP2020025344A (en) * 2019-11-15 2020-02-13 セイコーエプソン株式会社 Vibration element, vibrator, electronic device, electronic apparatus, mobile body, and manufacturing method of vibration element

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JP2013236290A (en) 2012-05-10 2013-11-21 Nippon Dempa Kogyo Co Ltd Crystal vibrating reed, crystal device, and method of manufacturing crystal vibrating reed
JP5637522B1 (en) 2014-06-20 2014-12-10 協同組合Ａｑｕｅｓ Algae inhibitor and its storage case / laying equipment

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5637522U (en) * 1979-08-28 1981-04-09
JP2005136575A (en) * 2003-10-29 2005-05-26 Seiko Epson Corp Piezoelectric vibrating piece, structure of excitation electrode thereof, electrode forming method, piezoelectric device, cellular telephone device employing piezoelectric device and electronic equipment employing piezoelectric device
WO2015004755A1 (en) * 2013-07-10 2015-01-15 株式会社シンクロン Optical film thickness measurement device, thin film forming device, and method for measuring film thickness
JP2020025344A (en) * 2019-11-15 2020-02-13 セイコーエプソン株式会社 Vibration element, vibrator, electronic device, electronic apparatus, mobile body, and manufacturing method of vibration element

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