JP4618787B2 - Electroplating solution evaluation apparatus and method - Google Patents

Electroplating solution evaluation apparatus and method Download PDF

Info

Publication number
JP4618787B2
JP4618787B2 JP2005025247A JP2005025247A JP4618787B2 JP 4618787 B2 JP4618787 B2 JP 4618787B2 JP 2005025247 A JP2005025247 A JP 2005025247A JP 2005025247 A JP2005025247 A JP 2005025247A JP 4618787 B2 JP4618787 B2 JP 4618787B2
Authority
JP
Japan
Prior art keywords
electroplating solution
cell test
hull cell
cathode
evaluating
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.)
Expired - Fee Related
Application number
JP2005025247A
Other languages
Japanese (ja)
Other versions
JP2006214751A (en
Inventor
隆三 阿部
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.)
Tokin Corp
Original Assignee
NEC Tokin Corp
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 NEC Tokin Corp filed Critical NEC Tokin Corp
Priority to JP2005025247A priority Critical patent/JP4618787B2/en
Publication of JP2006214751A publication Critical patent/JP2006214751A/en
Application granted granted Critical
Publication of JP4618787B2 publication Critical patent/JP4618787B2/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Electroplating Methods And Accessories (AREA)

Description

本発明は、電気めっきに使用する電気めっき液の評価装置及びその評価方法に関するものである。   The present invention relates to an evaluation apparatus for an electroplating solution used for electroplating and an evaluation method thereof.

電気めっき液の評価方法の一つに、ハルセル試験法がある。ハルセル試験法とは、光沢剤等の添加剤濃度の適不適や電解条件等、電気めっき液の状態を評価することができるもので、このような評価方法の一例として、特許文献１に開示されている方法がある。図６は、特許文献１に開示されている従来の台形の形状をしたハルセル試験槽であり、図７に示すように電源、電流計、電圧計などを接続し、さらに加熱装置、攪拌装置等（図示せず）を備えた条件の下で評価試験が行われる。   One of the methods for evaluating the electroplating solution is the hull cell test method. The Hull cell test method is capable of evaluating the state of the electroplating solution, such as the suitability of the concentration of additives such as brighteners and electrolysis conditions, and is disclosed in Patent Document 1 as an example of such an evaluation method. There is a way. FIG. 6 is a conventional trapezoidal hull cell test tank disclosed in Patent Document 1, and is connected to a power source, an ammeter, a voltmeter, etc., as shown in FIG. An evaluation test is performed under conditions with (not shown).

ハルセル試験槽は陽極面と陰極面が平行になっておらず、図６のように陰極面が陽極面に対して傾斜している。このため、めっきを行うと、陽極面に近い方の陰極面の部分に流入する単位面積あたりの電流、即ち、電流密度は高く、陽極面に遠い方の陰極面の部分に行くに従って流入する電流密度は徐々に低くなる。したがって、ハルセル試験法により、電流密度の広範囲変化に対して陰極面に析出した金属皮膜の状態を観察することができる。例えば、光沢ニッケルめっき液の場合、光沢剤の過不足により低電流密度でのつきまわり不良や光沢不足、高電流密度部分でのピット、焼け又は密着不良が観察できる。   In the Hull cell test tank, the anode surface and the cathode surface are not parallel, and the cathode surface is inclined with respect to the anode surface as shown in FIG. For this reason, when plating is performed, the current per unit area that flows into the portion of the cathode surface closer to the anode surface, that is, the current that flows into the portion of the cathode surface that is higher in current density and farther from the anode surface. The density gradually decreases. Therefore, the state of the metal film deposited on the cathode surface can be observed with respect to a wide range of current density changes by the Hull cell test method. For example, in the case of a bright nickel plating solution, it is possible to observe poor throwing power at low current density, insufficient gloss, pits, burns or poor adhesion at high current density due to excessive or insufficient brightener.

特開平５−７２１６７号公報Japanese Patent Laid-Open No. 5-72167

電気めっき液の特性の一つに、つきまわり性と呼ばれる特性がある。それは低電流密度域、あるいは電気めっき液金属イオン濃度の低い領域でのめっきの付き易さのことで、例えば細長い筒状の被めっき物の筒内側へめっきする場合などは、つきまわり性の良い電気めっき液が求められる。しかしながら、特許文献１に記載されているハルセル試験法では、このつきまわり性の評価が出来ず、ハルセル試験片の状態を目視観察による判断にとどまり、正確に判断することができないという欠点があった。   One of the characteristics of the electroplating solution is a characteristic called throwing power. This means that the plating is easy in a low current density region or a region where the electroplating liquid metal ion concentration is low. For example, when plating inside a long cylindrical object to be plated, the throwing power is good. An electroplating solution is required. However, the Hull Cell test method described in Patent Document 1 has a drawback in that this throwing power cannot be evaluated, and the state of the Hull cell test piece is limited to visual observation and cannot be accurately determined. .

したがって、本発明の目的は、ハルセル試験法の特徴である広範囲な電流密度を利用することにより、電気めっき液のつきまわり性を評価することが出来る評価装置及びその評価方法を提供することにある。   Accordingly, an object of the present invention is to provide an evaluation apparatus that can evaluate the throwing power of an electroplating solution by utilizing a wide range of current density that is a feature of the Hull cell test method, and an evaluation method thereof. .

本発明は、前記課題の解決のため、電気めっき液の特性を評価する装置において、ハルセル試験槽に電気めっき液を入れ、ハルセル試験槽の陽極から陰極部に電気めっき液を通して電流を流し、前記電気めっき液のつきまわり性を評価するものであり、前記陰極部は、陰極となるハルセル試験片にスペーサーを介して前記電流の一部を遮断する遮蔽板を配したものであることを特徴とする電気めっき液の評価装置である。 The present invention is, for solving the above problems, an apparatus for evaluating the characteristics of the electroplating solution, put electroplating solution to Hull cell test chamber, passing a current through the electroplating solution to the cathode portion from the anode of the Hull cell test chamber, the it is intended to evaluate the throwing of electroplating solution, wherein the cathode part includes a feature that via a spacer Hull cell test specimen as a cathode is obtained by distributing the shielding plate for blocking a part of the current This is an electroplating solution evaluation apparatus.

また、電気めっき液の特性を評価する方法において、ハルセル試験槽に電気めっき液を入れ、ハルセル試験槽の陽極から陰極部に電気めっき液を通して電流を流し、前記陰極部に遮蔽板を配して流れる電流の一部を遮断することにより、前記電気めっき液のつきまわり性を評価する電気めっき液の評価方法であり、前記陰極部は、陰極となるハルセル試験片にスペーサーを介して前記遮蔽板を配したものであることを特徴とする電気めっき液の評価方法である。また、前記ハルセル試験片への遮蔽ラインを越えてめっき析出状態を観察することにより、前記電気めっき液のつきまわり性を評価することを特徴とする電気めっき液の評価方法である。 Further, in the method for evaluating the characteristics of the electroplating solution, the electroplating solution is put into a hull cell test tank, a current is passed through the electroplating solution from the anode to the cathode part of the hull cell test tank, and a shielding plate is arranged on the cathode part. by blocking a portion of the current flowing, said an evaluation method of an electroplating solution for evaluating the throwing of electroplating solution, wherein the cathode part, the shield plate via a spacer Hull cell test specimen as a cathode This is a method for evaluating an electroplating solution. Further, by observing the plating deposition state beyond the shielding lines to the Hull cell test specimen, the evaluation method of the electroplating solution and evaluating the throwing of the electroplating solution.

本発明によれば、前記の手段を採用することにより、簡便な方法で、かつ正確な評価ができる電気めっき液の評価装置及びその評価方法を提供することが可能となった。   According to the present invention, it is possible to provide an electroplating solution evaluation apparatus and an evaluation method thereof that can perform accurate evaluation by a simple method by employing the above-described means.

本発明に係る電気めっき液の評価装置と、その評価方法の実施の形態について、具体的な例を挙げて説明する。   Embodiments of the electroplating solution evaluation apparatus and the evaluation method according to the present invention will be described with specific examples.

図１は本発明によるハルセル試験装置を示す。試験装置には株式会社山本鍍金試験器のハルセル試験装置を用いた。この装置はハルセル試験槽１と陽極２と陰極部３から構成され、陰極部３は、遮蔽板４とハルセル試験片６との間隔を調整するスペーサー５と、遮蔽板４とスペーサー５とハルセル試験片６を固定する留め具７から成り、図７のように陽極２と陰極部３に接続される直流電源１７から構成されている。また、ハルセル試験槽内には、めっき液８がある。 FIG. 1 shows a hull cell test apparatus according to the present invention. As a test apparatus, a Hull cell test apparatus of Yamamoto Metal Testing Co., Ltd. was used. This apparatus comprises a hull cell test chamber 1, an anode 2, and a cathode part 3. The cathode part 3 includes a spacer 5 for adjusting the distance between the shielding plate 4 and the hull cell test piece 6, and the shielding plate 4, the spacer 5, and the hull cell test. It consists of a fastener 7 for fixing the piece 6 and is composed of a DC power source 17 connected to the anode 2 and the cathode part 3 as shown in FIG. There is a plating solution 8 in the hull cell test tank.

電気めっき液８は電解液で、金属イオンが溶解しており、電圧をかけると陽極２から金属イオンが電子を受け取って陰極部３表面に金属として析出するようになっている。ハルセル試験槽１は面状の陽極２に対して面状の陰極部３が平行ではなく斜めに配されているため、陰極部３の陽極２に近い部分ほど高電流密度状態となり、陰極部３の陽極２から遠い部分は低電流密度状態になる。 The electroplating solution 8 is an electrolytic solution in which metal ions are dissolved. When a voltage is applied, the metal ions receive electrons from the anode 2 and are deposited as metal on the surface of the cathode portion 3. For Hull cell test chamber 1 in which planar cathode part 3 with respect to planar anode 2 is disposed obliquely not parallel becomes a high current density state portion nearer to the anode 2 cathode 3, cathode part 3 The portion far from the anode 2 is in a low current density state.

図２にハルセル試験片６とスペーサー５と遮蔽板４の構成を示す。ハルセル試験片６からスペーサー５の分の隙間をあけて遮蔽板４を置いている。本発明の実施の形態では、スペーサー５の厚みは５０μｍとしたが、スペーサー５の厚みを変えることで、イオン供給量の調整ができるので、任意の厚みで評価してもよい。   FIG. 2 shows the configuration of the Hull cell test piece 6, the spacer 5, and the shielding plate 4. The shielding plate 4 is placed with a gap corresponding to the spacer 5 from the hull cell test piece 6. In the embodiment of the present invention, the thickness of the spacer 5 is 50 μm. However, since the ion supply amount can be adjusted by changing the thickness of the spacer 5, the thickness may be evaluated with an arbitrary thickness.

図３は、従来の遮蔽板がない場合の金属イオンの動きを示す模式図である。遮蔽板がない場合には、金属イオン１２は遮断されないがため、陰極部のハルセル試験片６に次々に析出していく。   FIG. 3 is a schematic diagram showing the movement of metal ions when there is no conventional shielding plate. When there is no shielding plate, the metal ions 12 are not blocked, and thus deposit one after another on the Hull cell test piece 6 in the cathode portion.

一方、図４は、本発明の遮蔽板がある場合の金属イオンの動きを示す模式図である。遮蔽板４がある場合には、初期に遮蔽板４とハイセル試験片６の間にあった金属イオン１２がハルセル試験片６の表面に析出した後、金属イオン１２の供給は、遮蔽板４とハルセル試験片６の隙間に限定されるため、難しくなってくる。その結果、電気めっき液の粘度、金属イオン濃度、添加剤の種類などによって、金属イオン供給能力に差が生じ、ハルセル試験片６へのめっき析出状態を観察することにより、電気めっき液のつきまわり性の評価が出来ることになる。   On the other hand, FIG. 4 is a schematic diagram showing the movement of metal ions when there is a shielding plate of the present invention. When the shielding plate 4 is present, after the metal ions 12 that were initially between the shielding plate 4 and the high cell test piece 6 are deposited on the surface of the hull cell test piece 6, the metal ions 12 are supplied to the shield plate 4 and the hull cell test. Since it is limited to the gap of the piece 6, it becomes difficult. As a result, the metal ion supply capacity varies depending on the viscosity, metal ion concentration, additive type, etc. of the electroplating solution, and by observing the plating deposition state on the Hull cell test piece 6, The sex can be evaluated.

図５にハルセル試験片６の遮蔽部分のめっき析出例を示す。遮蔽ライン１０は、遮蔽板４によって遮蔽された部分とされない部分の境界を示す。遮蔽ライン１０からはみ出した部分がつきまわり性評価部分１１である。表１にニッケルめっき浴のワット浴とスルファミン酸浴との比較評価結果を示す。めっき条件は電流０．５アンペア、めっき時間３分、撹拌なし、浴温は５０℃で、評価項目は遮蔽された部分にめっきされたつきまわり性評価部分１１の長さを測定した。   FIG. 5 shows an example of plating deposition on the shielding portion of the hull cell test piece 6. The shielding line 10 indicates a boundary between a portion that is not covered by the shielding plate 4 and a portion that is not covered. A portion protruding from the shielding line 10 is a throwing power evaluation portion 11. Table 1 shows the results of comparative evaluation between the watt bath and the sulfamic acid bath of the nickel plating bath. The plating conditions were a current of 0.5 ampere, a plating time of 3 minutes, no stirring, a bath temperature of 50 ° C., and the evaluation item was the length of the throwing power evaluation portion 11 plated on the shielded portion.

Figure 0004618787
Figure 0004618787

表１より、スルファミン酸浴の方がワット浴に比較して、つきまわり性が良い電気めっき液であるということが確認できた。   From Table 1, it was confirmed that the sulfamic acid bath is an electroplating solution having better throwing power than the Watt bath.

本発明での遮蔽物は、板状で方形の遮蔽板を使用したが、評価目的によっては、網状、パンチングプレート状などを選択することもある。   As the shield in the present invention, a plate-shaped and square shield plate is used. However, depending on the evaluation purpose, a mesh shape, a punching plate shape, or the like may be selected.

本発明の実施の形態に係るハルセル試験装置を示す斜視図。1 is a perspective view showing a hull cell testing apparatus according to an embodiment of the present invention. 本発明の実施の形態に係る陰極部のハルセル試験片とスペーサーと遮蔽板を示す構成図。The block diagram which shows the hull cell test piece of the cathode part which concerns on embodiment of this invention, a spacer, and a shielding board. 従来の遮蔽板がない場合の金属イオンの動きを示す模式図。The schematic diagram which shows the motion of the metal ion when there is no conventional shielding board. 本発明の実施の形態に係る遮蔽板がある場合の金属イオンの動きを示す模式図。The schematic diagram which shows the motion of a metal ion when there exists a shielding board which concerns on embodiment of this invention. 本発明の実施例に係るハルセル試験片の遮蔽部分のめっき析出を示す概略図。Schematic which shows plating deposition of the shielding part of the hull cell test piece which concerns on the Example of this invention. 従来のハルセル試験槽の斜視図。The perspective view of the conventional hull cell test tank. ハルセル試験槽の電気接続を示す概略図。Schematic which shows the electrical connection of a hull cell test tank.

符号の説明Explanation of symbols

１ ハルセル試験槽
２ 陽極
３ 陰極部
４ 遮蔽板
５ スペーサー
６ ハルセル試験片
７ 留め具
８ 電気めっき液
９ めっき部
１０ 遮蔽ライン
１１ つきまわり性評価部分
１２ 金属イオン
１３ 電子
１４ 電圧計
１５ 電流計
１６ 摺動抵抗
１７ 直流電源 DESCRIPTION OF SYMBOLS 1 Hull cell test tank 2 Anode 3 Cathode part 4 Shielding plate 5 Spacer 6 Hull cell test piece 7 Fastener 8 Electroplating solution 9 Plating part 10 Shielding line 11 Throwing property evaluation part 12 Metal ion 13 Electron 14 Voltmeter 15 Ammeter 16 Sliding Dynamic resistance 17 DC power supply

Claims (3)

電気めっき液の特性を評価する装置において、ハルセル試験槽に電気めっき液を入れ、前記ハルセル試験槽の陽極から陰極部に前記電気めっき液を通して電流を流し、前記電気めっき液のつきまわり性を評価するものであり、前記陰極部は、陰極となるハルセル試験片にスペーサーを介して前記電流の一部を遮断する遮蔽板を配したものであることを特徴とする電気めっき液の評価装置。 In the apparatus for evaluating the characteristics of the electroplating solution, the electroplating solution is put into the hull cell test tank, the current is passed through the electroplating solution from the anode to the cathode part of the hull cell test tank, and the throwing power of the electroplating solution is evaluated. is intended to, the cathode unit, the evaluation device of the electroplating solution, characterized in that via a spacer Hull cell test specimen as a cathode is obtained by distributing the shielding plate for blocking a part of said current. 電気めっき液の特性を評価する方法において、ハルセル試験槽に電気めっき液を入れ、前記ハルセル試験槽の陽極から陰極部に前記電気めっき液を通して電流を流し、前記陰極部に遮蔽板を配して流れる電流の一部を遮断させることにより、前記電気めっき液のつきまわり性を評価する方法であり、前記陰極部は、陰極となるハルセル試験片にスペーサーを介して前記遮蔽板を配したものであることを特徴とする電気めっき液の評価方法。 In the method of evaluating the characteristics of the electroplating solution, the electroplating solution is put into a hull cell test tank, a current is passed through the electroplating solution from the anode to the cathode part of the hull cell test tank, and a shielding plate is arranged on the cathode part. by blocking a portion of the current flowing is a method of evaluating the throwing of the electroplating solution, the cathode unit, which was arranged the shielding plate via a spacer Hull cell test specimen as a cathode A method for evaluating an electroplating solution, comprising: 前記ハルセル試験片への遮蔽ラインを越えてめっき析出状態を観察することにより、前記電気めっき液のつきまわり性を評価することを特徴とする請求項２に記載の電気めっき液の評価方法。 The method for evaluating an electroplating solution according to claim 2 , wherein the throwing power of the electroplating solution is evaluated by observing the plating deposition state beyond the shielding line to the Hull cell test piece.
JP2005025247A 2005-02-01 2005-02-01 Electroplating solution evaluation apparatus and method Expired - Fee Related JP4618787B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP2005025247A JP4618787B2 (en) 2005-02-01 2005-02-01 Electroplating solution evaluation apparatus and method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP2005025247A JP4618787B2 (en) 2005-02-01 2005-02-01 Electroplating solution evaluation apparatus and method

Publications (2)

Publication Number Publication Date
JP2006214751A JP2006214751A (en) 2006-08-17
JP4618787B2 true JP4618787B2 (en) 2011-01-26

Family

ID=36978119

Family Applications (1)

Application Number Title Priority Date Filing Date
JP2005025247A Expired - Fee Related JP4618787B2 (en) 2005-02-01 2005-02-01 Electroplating solution evaluation apparatus and method

Country Status (1)

Country Link
JP (1) JP4618787B2 (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP5114271B2 (en) * 2008-03-31 2013-01-09 メタローテクノロジーズジャパン株式会社 Around plating evaluation apparatus and evaluation method
CN103173842B (en) * 2013-02-25 2016-03-30 上海大学 The device of electroplating technology and electroplate liquid development experiments is carried out under hyperbaric environment
CN108385157B (en) * 2018-06-04 2023-07-07 电子科技大学 Electroplating solution dispersion capability evaluation device and evaluation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55112253U (en) * 1979-01-31 1980-08-07
JPS57182963U (en) * 1981-05-18 1982-11-19
JPS6195242A (en) * 1984-10-16 1986-05-14 Toyota Motor Corp Method for evaluation test of electroplating solution
JPH0572167A (en) * 1991-09-12 1993-03-23 Sumitomo Metal Mining Co Ltd Control method for composition of electrolytic solution

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55112253U (en) * 1979-01-31 1980-08-07
JPS57182963U (en) * 1981-05-18 1982-11-19
JPS6195242A (en) * 1984-10-16 1986-05-14 Toyota Motor Corp Method for evaluation test of electroplating solution
JPH0572167A (en) * 1991-09-12 1993-03-23 Sumitomo Metal Mining Co Ltd Control method for composition of electrolytic solution

Also Published As

Publication number Publication date
JP2006214751A (en) 2006-08-17

Similar Documents

Publication Publication Date Title
CN102597321B (en) Coated articles and methods
Pecequilo et al. Study of copper electrodeposition mechanism from a strike alkaline bath prepared with 1-hydroxyethane-1, 1-diphosphonic acid through cyclic voltammetry technique
Hansal et al. Pulse-electrodeposited NiP–SiC composite coatings
de Almeida et al. Electrodeposition of CuZn films from free-of-cyanide alkaline baths containing EDTA as complexing agent
Zhang et al. Electrodeposit copper from alkaline cyanide-free baths containing 5, 5′-dimethylhydantoin and citrate as complexing agents
CN104911648A (en) Cyanide-free acidic matte silver electroplating compositions and methods
JP4618787B2 (en) Electroplating solution evaluation apparatus and method
Böck et al. Effect of additive and current mode on surface morphology of palladium films from a non-aqueous deep eutectic solution (DES)
Karami et al. Electroplating nanostructured hard gold through the pulse galvanostatic method
US20210254230A1 (en) Silver electrolyte for depositing dispersion silver layers and contact surfaces with dispersion silver layers
Li et al. Effect of Saccharin on the process and properties of nickel electrodeposition from sulfate electrolyte
Mariani et al. A systematic study of pulse and pulse reverse plating on acid copper bath for decorative and functional applications
Dimitrijević et al. Temperature effect on decorative gold coatings obtained from electrolyte based on mercaptotriazole–comparison with cyanide
Cârâc et al. Effect of nano-Al 2 O 3 particles and of the Co concentration on the corrosion behavior of electrodeposited Ni–Co alloys
Veilleux et al. Influence of gelatin on deposit morphology during copper electrorefining using scaled industrial cells
Nor et al. Electrodeposition of Co-Ni-Fe thin film using hull cell
JP6011874B2 (en) Method for evaluating inhibitors contained in plating solution
Rao et al. Magnetically induced codeposition of Ni–Cd alloy coatings for better corrosion protection
Török et al. Direct cathodic deposition of copper on steel wires from pyrophosphate baths
Vasilache et al. Studies of hardness for the electrodeposited nickel from watts baths with addition of polyvinyl pyrrolidone (PVP)
Dela Pena Electrodeposition of copper using additive-containing low metal ion concentration electrolytes for Enface applications
Grill et al. Preparation and investigation of combinatorially electrodeposited zinc–nickel, zinc–cobalt, and zinc–nickel–cobalt material libraries
RU2784898C1 (en) Modified hull cell for electroplating and potentiostatic electrolysis modes
Sherwin et al. Investigation on the effect of nickel and nickel-chromium alloy pulse current plating on copper substrate
Elias et al. Development of Ni-P alloy coatings for better corrosion protection using glycerol as additive

Legal Events

Date Code Title Description
A621 Written request for application examination

Free format text: JAPANESE INTERMEDIATE CODE: A621

Effective date: 20071010

A977 Report on retrieval

Free format text: JAPANESE INTERMEDIATE CODE: A971007

Effective date: 20100401

A131 Notification of reasons for refusal

Free format text: JAPANESE INTERMEDIATE CODE: A131

Effective date: 20100804

A521 Written amendment

Free format text: JAPANESE INTERMEDIATE CODE: A523

Effective date: 20100924

TRDD Decision of grant or rejection written
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20101020

A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

A61 First payment of annual fees (during grant procedure)

Free format text: JAPANESE INTERMEDIATE CODE: A61

Effective date: 20101025

FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20131105

Year of fee payment: 3

R150 Certificate of patent or registration of utility model

Free format text: JAPANESE INTERMEDIATE CODE: R150

LAPS Cancellation because of no payment of annual fees