JPH05166794A - Substrate pretreatment method in forming film by sputtering - Google Patents
Substrate pretreatment method in forming film by sputteringInfo
- Publication number
- JPH05166794A JPH05166794A JP32750291A JP32750291A JPH05166794A JP H05166794 A JPH05166794 A JP H05166794A JP 32750291 A JP32750291 A JP 32750291A JP 32750291 A JP32750291 A JP 32750291A JP H05166794 A JPH05166794 A JP H05166794A
- Authority
- JP
- Japan
- Prior art keywords
- film
- substrate
- sputtering
- ceramic substrate
- pretreatment method
- 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
Links
- 239000000758 substrate Substances 0.000 title claims abstract description 33
- 238000004544 sputter deposition Methods 0.000 title claims abstract description 10
- 238000002203 pretreatment Methods 0.000 title claims description 9
- 239000000919 ceramic Substances 0.000 claims abstract description 15
- 238000005530 etching Methods 0.000 claims abstract description 13
- YUOWTJMRMWQJDA-UHFFFAOYSA-J tin(iv) fluoride Chemical compound [F-].[F-].[F-].[F-].[Sn+4] YUOWTJMRMWQJDA-UHFFFAOYSA-J 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 239000000470 constituent Substances 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 24
- 239000011651 chromium Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 9
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 8
- 239000007789 gas Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 238000004506 ultrasonic cleaning Methods 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000005684 electric field Effects 0.000 description 2
- 239000010931 gold Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
Landscapes
- Physical Vapour Deposition (AREA)
- Weting (AREA)
- Physical Deposition Of Substances That Are Components Of Semiconductor Devices (AREA)
Abstract
(57)【要約】
【目的】 セラミックス基板上に密着強度の高い電極膜
を形成する。
【構成】 スパッタ前のセラミックス基板１をフッ化ス
ズ溶液に浸漬することによりセラミックス基板１の構成
粒子の表面に均一にエッチング痕２を生じさせ、その上
にスパッタされるCr膜３がエッチング痕に浸入する。
(57) [Abstract] [Purpose] To form an electrode film with high adhesion strength on a ceramic substrate. [Structure] By immersing the ceramic substrate 1 before sputtering in a tin fluoride solution, an etching mark 2 is uniformly formed on the surface of the constituent particles of the ceramic substrate 1, and the Cr film 3 sputtered on the etching mark 2 becomes an etching mark. Infiltrate.
Description
【０００１】[0001]
【産業上の利用分野】本発明は、例えば圧電素子上の電
極作成のための、スパッタ成膜による薄膜作製時のスパ
ッタ成膜時基板前処理法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a substrate pretreatment method during sputtering film formation during thin film formation by sputtering film formation, for example, for forming electrodes on a piezoelectric element.
【０００２】[0002]
【従来の技術】従来、スパッタ法にて成膜を行なうセラ
ミックス基板の前工程としては、基板を真空槽内に挿入
した後、Ａｒ（アルゴン）ガスを真空槽内に導入して電
場により電離させ、その電離気体を基板表面に衝突させ
て、基板表面に付着した汚染物質をたたき出す逆スパッ
タ法などのドライプロセスにより、表面の汚染物質を除
去するのが一般的であった。スパッタ法とは、素子基板
を、電極材を構成する物質のターゲットを備えた真空槽
内に挿入し、Ａｒガスを導入したのち電場を印加して、
ガスの電離気体の粒子をターゲットに衝突させることに
より電極構成物質の粒子をたたき出し、対向して置かれ
た素子基板上に堆積させて電極薄膜を作成する方法であ
る。2. Description of the Related Art Conventionally, as a pre-process of a ceramic substrate for forming a film by a sputtering method, after inserting the substrate into a vacuum chamber, Ar (argon) gas is introduced into the vacuum chamber and ionized by an electric field. It was common to remove surface contaminants by a dry process such as a reverse sputtering method in which the ionized gas is made to collide with the substrate surface to knock out the contaminants adhering to the substrate surface. With the sputtering method, the element substrate is inserted into a vacuum chamber provided with a target of a substance forming an electrode material, Ar gas is introduced, and then an electric field is applied.
This is a method in which particles of an electrode constituent substance are knocked out by colliding particles of a gas ionized gas with a target, and the particles are deposited on the element substrates placed facing each other to form an electrode thin film.
【０００３】[0003]
【発明が解決しようとする課題】しかしながら、従来法
では被膜の残留応力による基板との密着強度の低下を防
ぐのに十分な効果は得られず、従来技術により作成した
電極膜の密着強度を引き剥し法で評価したときの値は３
０〜５０kg/cm2程度と非常に低い値であった。However, the conventional method is not sufficiently effective in preventing the reduction of the adhesion strength with the substrate due to the residual stress of the coating film, and the adhesion strength of the electrode film prepared by the conventional technique is reduced. The value when evaluated by the peeling method is 3
It was a very low value of 0 to 50 kg / cm 2 .
【０００４】本発明は、上述した問題点を解決するため
になされたものであり、密着強度の高いスパッタ膜を得
る前処理法を提供することを目的としている。The present invention has been made to solve the above-mentioned problems, and an object thereof is to provide a pretreatment method for obtaining a sputtered film having high adhesion strength.
【０００５】[0005]
【課題を解決するための手段】この目的を達成するため
に本発明の前処理法は、フッ化スズ溶液によるエッチン
グ工程を有している。In order to achieve this object, the pretreatment method of the present invention includes an etching step using a tin fluoride solution.
【０００６】[0006]
【作用】上記の構成を有する本発明の前処理法は、スパ
ッタ前の基板をフッ化スズ溶液に浸漬することにより基
板表面をエッチングし、基板表面に均一にエッチング痕
を生じさせる。In the pretreatment method of the present invention having the above structure, the surface of the substrate before etching is immersed in a tin fluoride solution to etch the surface of the substrate, thereby uniformly forming etching marks on the surface of the substrate.
【０００７】[0007]
【実施例】以下、本発明を具体化した一実施例を図面を
参照して説明する。DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to the drawings.
【０００８】まず、図１を参照して本発明の前処理法を
用いて作製した電極膜の構成を説明すると、PbZrO3（ジ
ルコン酸鉛）-PbTiO3（チタン酸鉛）系のセラミックス
基板１はPbZrO3 及びPbTiO3の粒子よりなり、基板の表
面全体に均一にエッチング痕２が生じている。基板上に
堆積させられた Cr（クロム）膜３はそのエッチング痕
２にも浸入しており、Cr膜３の上にはさらに Ni（ニッ
ケル）膜４が堆積させられている。First, referring to FIG. 1, the structure of an electrode film produced by the pretreatment method of the present invention will be described. A PbZrO 3 (lead zirconate) -PbTiO 3 (lead titanate) ceramic substrate 1 will be described. Is composed of particles of PbZrO 3 and PbTiO 3 , and etching marks 2 are uniformly formed on the entire surface of the substrate. The Cr (chromium) film 3 deposited on the substrate has also penetrated into the etching mark 2, and the Ni (nickel) film 4 is further deposited on the Cr film 3.
【０００９】次に、図２〜図４を参照して本実施例の電
極膜の製造工程を説明する。Next, the manufacturing process of the electrode film of this embodiment will be described with reference to FIGS.
【００１０】最初にセラミックス基板１は図２（ａ）の
ように溶剤洗浄用ビーカ５中のアセトン６に浸され、超
音波洗浄器７により超音波洗浄を５分間施される。つい
で、図２（ｂ）のようにエアースプレー８のエアーブロ
ーにより強制乾燥された後、図２（ｃ）に示すように恒
温槽９によって６０℃に保たれたアルカリ脱脂液アルプ
レップ（奥野製薬社製）１０にて５分間脱脂が行われ
る。続いて、図２（ｄ）のように超音波洗浄器７により
純水１１中にて超音波洗浄を１０分間行なった後、図２
（ｅ）のように室温中に置かれたフッ化スズ溶液１２に
１５分間浸漬される。次に図２（ｆ）のように水洗槽１
３にて１分間洗浄され、前処理工程は終了する。前処理
が終了した時点で図３のようにセラミックス基板１の表
面にはエッチング痕２が生じている。その後セラミック
ス基板１は図４に示すように、スパッタ装置の真空槽１
４に搬入され、Crターゲット１５、Niターゲット１６の
順にスパッタされて、セラミックス基板１の上にCr膜
３、Ni膜４が堆積させられる。Cr膜３はエッチング痕２
に浸入しアンカー効果により密着強度が向上する。First, the ceramic substrate 1 is immersed in acetone 6 in a beaker 5 for solvent cleaning as shown in FIG. 2 (a), and ultrasonic cleaning is performed by an ultrasonic cleaning device 7 for 5 minutes. Then, as shown in FIG. 2 (b), after being forcedly dried by the air blow of the air spray 8, as shown in FIG. 2 (c), the alkaline degreasing liquid Alprep (Okuno Pharmaceutical Co. (Manufactured) 10 for 5 minutes. Subsequently, as shown in FIG. 2D, ultrasonic cleaning is performed in pure water 11 by the ultrasonic cleaning device 7 for 10 minutes, and then, as shown in FIG.
As in (e), it is immersed in the tin fluoride solution 12 placed at room temperature for 15 minutes. Next, as shown in FIG. 2 (f), the washing tank 1
The cleaning process is finished for 1 minute at 3, and the pretreatment process is completed. When the pretreatment is completed, etching marks 2 are formed on the surface of the ceramic substrate 1 as shown in FIG. After that, the ceramic substrate 1 is, as shown in FIG.
Then, the Cr target 15 and the Ni target 16 are sputtered in this order, and the Cr film 3 and the Ni film 4 are deposited on the ceramic substrate 1. Cr film 3 has etching marks 2
And the anchor effect improves the adhesion strength.
【００１１】得られた電極膜の密着強度を引き剥し法で
評価した結果を表１に示す。Table 1 shows the results of evaluation of the adhesion strength of the obtained electrode film by the peeling method.
【００１２】[0012]
【表１】 [Table 1]
【００１３】このように、本実施例の前処理法により約
９９ｋｇ／ｃｍ2の高い密着強度が得られていることが
わかる。密着強度の高い膜は電極としての信頼性を高め
ることができるため、本実施例の前処理法により信頼性
に優れた電極膜を得ることができる。As described above, it can be seen that a high adhesion strength of about 99 kg / cm 2 was obtained by the pretreatment method of this embodiment. Since the film having high adhesion strength can improve the reliability as an electrode, the electrode film having excellent reliability can be obtained by the pretreatment method of this embodiment.
【００１４】本発明は、以上詳述した実施例に限定され
ることなく、その主旨を逸脱しない範囲において種々の
変更を加えることができる。例えば、本実施例ではセラ
ミックス基板をフッ化スズ溶液に浸すことにより処理を
行っているが、この行程をスプレーによるフッ化スズ溶
液の吹き付けとする、あるいは刷毛によりセラミックス
基板上にフッ化スズ溶液を塗布するとすることも可能で
ある。また、本実施例では、スパッタを行う薄膜を一層
目Cr膜、二層目Ni膜としたが、これをTi（チタン）,Cu
（銅）,Al（アルミニウム）,Au（金）,Ag（銀）及びそ
の合金とすることも可能であり、さらに電極用途ではな
く、装飾、耐蝕、耐摩耗用の金属膜、酸化物膜とするこ
とも可能である。The present invention is not limited to the embodiments described in detail above, and various modifications can be made without departing from the spirit of the invention. For example, in this embodiment, the treatment is performed by immersing the ceramics substrate in the tin fluoride solution, but this process is performed by spraying the tin fluoride solution by spraying, or by brushing the tin fluoride solution on the ceramics substrate. It is also possible to apply. In addition, in the present embodiment, the thin film to be sputtered was the first layer Cr film and the second layer Ni film.
It is also possible to use (copper), Al (aluminum), Au (gold), Ag (silver) and their alloys, and also for decoration, corrosion resistance, abrasion resistance metal film and oxide film, not for electrode use. It is also possible to do so.
【００１５】[0015]
【発明の効果】以上説明したことから明かなように、フ
ッ化スズ溶液によりセラミックス基板表面をエッチング
することにより、セラミックス基板上に密着性の高いス
パッタ膜を得ることが出来る。As is apparent from the above description, by etching the surface of the ceramic substrate with the tin fluoride solution, a sputtered film having high adhesion can be obtained on the ceramic substrate.
【図１】図１は本発明を適用した一実施例の電極の断面
図である。FIG. 1 is a cross-sectional view of an electrode of an embodiment to which the present invention is applied.
【図２】図２（ａ）〜（ｆ）は本実施例の電極基板の前
処理工程を順に示す説明図である。2A to 2F are explanatory views sequentially showing a pretreatment process of the electrode substrate of the present embodiment.
【図３】図３は本実施例の前処理後の基板の断面図であ
る。FIG. 3 is a cross-sectional view of the substrate after the pretreatment of this embodiment.
【図４】図４は本実施例の電極のスパッタ工程を示す説
明図である。FIG. 4 is an explanatory view showing an electrode sputtering process of the present embodiment.
１ セラミックス基板 ２ エッチング痕 ３ Cr膜 ４ Ni膜 ５ 溶剤洗浄用ビーカ ６ アセトン ７ 超音波洗浄器 ８ エアースプレー ９ 恒温槽 １０ アルカリ脱脂液アルプレップ １１ 純水 １２ フッ化スズ溶液 １３ 水洗槽 １４ 真空槽 １５ Crターゲット １６ Niターゲット 1 Ceramics Substrate 2 Etching Trace 3 Cr Film 4 Ni Film 5 Solvent Cleaning Beaker 6 Acetone 7 Ultrasonic Cleaner 8 Air Spray 9 Constant Temperature Bath 10 Alkaline Degreasing Solution Alprep 11 Pure Water 12 Tin Fluoride Solution 13 Water Washing Bath 14 Vacuum Vessel 15 Cr target 16 Ni target
Claims (1)
の成膜の前処理として、フッ化スズ溶液により基板表面
をエッチングし基板表面に均一にエッチング痕を生じさ
せることを特徴とするスパッタ成膜時基板前処理法1. A substrate during sputtering film formation, characterized in that the substrate surface is etched with a tin fluoride solution to form etching marks uniformly on the substrate surface as a pretreatment for film formation on a ceramic substrate by the sputtering method. Pretreatment method
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32750291A JPH05166794A (en) | 1991-12-11 | 1991-12-11 | Substrate pretreatment method in forming film by sputtering |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32750291A JPH05166794A (en) | 1991-12-11 | 1991-12-11 | Substrate pretreatment method in forming film by sputtering |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH05166794A true JPH05166794A (en) | 1993-07-02 |
Family
ID=18199862
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32750291A Pending JPH05166794A (en) | 1991-12-11 | 1991-12-11 | Substrate pretreatment method in forming film by sputtering |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH05166794A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6419804B1 (en) * | 2000-11-22 | 2002-07-16 | Hsu Cheng-Shen | Contamination-resistant thin film deposition method |
| JP2010285288A (en) * | 2009-06-09 | 2010-12-24 | Panasonic Corp | Crystal manufacturing method and crystal manufacturing apparatus |
| US8492186B2 (en) | 2006-12-22 | 2013-07-23 | Toyoda Gosei Co., Ltd. | Method for producing group III nitride semiconductor layer, group III nitride semiconductor light-emitting device, and lamp |
| CN113414178A (en) * | 2021-06-29 | 2021-09-21 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic parts |
-
1991
- 1991-12-11 JP JP32750291A patent/JPH05166794A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6419804B1 (en) * | 2000-11-22 | 2002-07-16 | Hsu Cheng-Shen | Contamination-resistant thin film deposition method |
| US8492186B2 (en) | 2006-12-22 | 2013-07-23 | Toyoda Gosei Co., Ltd. | Method for producing group III nitride semiconductor layer, group III nitride semiconductor light-emitting device, and lamp |
| JP2010285288A (en) * | 2009-06-09 | 2010-12-24 | Panasonic Corp | Crystal manufacturing method and crystal manufacturing apparatus |
| CN113414178A (en) * | 2021-06-29 | 2021-09-21 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic parts |
| WO2023274009A1 (en) * | 2021-06-29 | 2023-01-05 | 北京北方华创微电子装备有限公司 | Method for cleaning ceramic part |
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