JPH06264256A - Steel excellent in weather resistance - Google Patents

Steel excellent in weather resistance

Info

Publication number
JPH06264256A
JPH06264256A JP5248693A JP5248693A JPH06264256A JP H06264256 A JPH06264256 A JP H06264256A JP 5248693 A JP5248693 A JP 5248693A JP 5248693 A JP5248693 A JP 5248693A JP H06264256 A JPH06264256 A JP H06264256A
Authority
JP
Japan
Prior art keywords
rust
steel
grain size
feooh
corrosion
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
JP5248693A
Other languages
Japanese (ja)
Other versions
JP2765425B2 (en
Inventor
Masato Yamashita
正人 山下
Hideaki Yuki
英昭 幸
Shunpei Misawa
俊平 三澤
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.)
Nippon Steel Corp
Original Assignee
Sumitomo Metal Industries Ltd
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
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=12916050&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=JPH06264256(A) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Sumitomo Metal Industries Ltd filed Critical Sumitomo Metal Industries Ltd
Priority to JP5248693A priority Critical patent/JP2765425B2/en
Publication of JPH06264256A publication Critical patent/JPH06264256A/en
Application granted granted Critical
Publication of JP2765425B2 publication Critical patent/JP2765425B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Chemical Treatment Of Metals (AREA)

Abstract

PURPOSE:To obtain high weather resistant steel excellent in sea salt resistance by coating the surface of steel with a rust layer or alpha-FeOOH having a specified average grain size. CONSTITUTION:The surface of the steel of low alloy steel or carbon steel such as weather resistant steel is coated with a rust layer having <=200nm average grain size or alpha-FeOOH having <=200nm average grain size. In this place, rust denotes a corrosion product in which alpha-FeOOH, gamma-FeOOH, Fe3O4 or the like caused by the atmospheric corrosion of general iron are coexistent unless the antibiotics are not specified, and if only the grain size is <=1200nm, the corrosion preventing properties of rust is good not only in an industrial area and a country area but also in a seaside area which is a severest environment in which sea salt grains are flying. In this way, the steel having high corrosion preventing properties in which the generation of the loose scale and flowing rust of red rust, yellow rust or the like in an atomospheric corrosion environment is eliminated can be obtd.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【産業上の利用分野】本発明は、耐候性に優れた鋼材、
特に鋼の耐候性に悪影響を及ぼす海塩粒子が飛来するよ
うな最も厳しい大気腐食環境中でさえも、安定で防食性
の高い錆に表面が覆われた耐候性の優れた鋼材に関する
ものである。
The present invention relates to a steel material having excellent weather resistance,
Particularly, the present invention relates to a steel material with excellent weather resistance whose surface is covered with rust that is stable and has high anticorrosiveness even in the most severe atmospheric corrosion environment where sea salt particles that adversely affect the weather resistance of steel come in. .

【0002】[0002]

【従来の技術】一般に鋼にP,Cu,Cr,Ni等の元素を添加す
ることにより、大気中における耐食性を向上させること
ができる。これらの低合金鋼は耐候性鋼と呼ばれるが、
屋外において数年で腐食に対して保護性のある錆(以下
耐候性錆という)を形成し、以後塗装等の耐食処理作業
を不要とするいわゆるメインテナンスフリー鋼である。
2. Description of the Related Art Generally, by adding elements such as P, Cu, Cr and Ni to steel, corrosion resistance in the atmosphere can be improved. These low alloy steels are called weather resistant steels,
It is a so-called maintenance-free steel that forms rust that protects against corrosion (hereinafter referred to as weather-resistant rust) in a few years outdoors and does not require subsequent corrosion-resistant treatment such as painting.

【0003】しかしながら、耐候性錆が形成されるまで
に数年かかるため、それまでの期間中に赤錆や黄錆等の
浮き錆や、流れ錆を生じてしまい、外見的に好ましくな
いばかりでなく周囲環境の汚染原因にもなるという問題
点を残している。
However, since it takes several years until the weather-resistant rust is formed, floating rust such as red rust and yellow rust and flow rust are generated during the period until then, and not only it is not preferable in appearance. The problem remains that it also causes pollution of the surrounding environment.

【0004】この問題については、たとえば特開平1-14
2088号にあるように、リン酸塩皮膜を形成させる表面処
理方法が提案されている。
Regarding this problem, for example, Japanese Patent Laid-Open No. 1-14
As in 2088, a surface treatment method for forming a phosphate film has been proposed.

【0005】[0005]

【発明が解決しようとする課題】しかし、リン酸塩皮膜
を形成させる以前に適当な前処理を施す必要がある等処
理の内容が複雑であり、また鋼材の溶接が必要な場合は
溶接部に処理を施すことは容易ではなく、建築構造物に
は適用が困難である等の問題がある。
However, the content of the treatment is complicated, such as the necessity of performing an appropriate pretreatment before forming the phosphate film, and when the welding of steel materials is required, It is not easy to apply the treatment and there is a problem that it is difficult to apply it to a building structure.

【0006】また、従来より耐候性鋼の表面に塗膜を施
すことや、リン酸塩皮膜を形成させたうえで塗装を施す
等の酔う面処理方法が行われているが、塗装により耐候
性錆の生成が遅くなり、また塗膜自体が劣化し外観を著
しく損ねる等の問題がある。
Conventionally, a drunk surface treatment method such as applying a coating film on the surface of weather resistant steel or applying a coating after forming a phosphate film has been used. There are problems that the generation of rust becomes slower, and the coating film itself deteriorates and the appearance is significantly impaired.

【0007】さらに、海塩粒子が飛来する海岸地帯など
厳しい環境では耐候性錆が形成されないという問題があ
る。
Further, there is a problem that weather resistant rust is not formed in a severe environment such as a coastal area where sea salt particles fly.

【0008】したがって、本発明の課題は、赤錆や黄錆
等の浮き錆や流れ錆を生じることがなく、人工的に早期
に育成した防食性に優れた錆層に覆われ耐海塩粒子性に
優れ耐候性の高い土木建築用等に用いる鋼材を提供する
ことである。
Therefore, the object of the present invention is to prevent sea rust such as red rust or yellow rust or flow rust, and to cover the sea salt particle resistance covered by a rust layer which is artificially grown early and has excellent corrosion resistance. An object of the present invention is to provide a steel material excellent in weather resistance and used for civil engineering and construction.

【0009】[0009]

【課題を解決するための手段】本発明者らは、鋼材表面
が一定の大きさ以下の平均結晶粒径を有する錆層で覆わ
れており、特に一定の大きさ以下の平均結晶粒径を有す
る錆がα−FeOOH であれば鋼材の耐候性が極めて高いこ
とを知見した。
Means for Solving the Problems The present inventors have found that the surface of a steel material is covered with a rust layer having an average crystal grain size of a certain size or less, and particularly the average grain size of a certain size or less is It was found that if the rust contained is α-FeOOH, the weather resistance of the steel material is extremely high.

【0010】すなわち、本願は、次記の発明を包含する
ものである。 1.鋼材表面が平均結晶粒径 200nm以下の錆層で覆わ
れていることを特徴とする耐候性に優れた鋼材。
That is, the present application includes the following inventions. 1. Steel material with excellent weather resistance, characterized in that the surface of the steel material is covered with a rust layer having an average crystal grain size of 200 nm or less.

【0011】2.鋼材表面が平均結晶粒径 200nm以下
のα−FeOOH で覆われていることを特徴とする耐候性に
優れた鋼材。
2. Steel material with excellent weather resistance, characterized in that the surface of the steel material is covered with α-FeOOH having an average crystal grain size of 200 nm or less.

【0012】[0012]

【作用】以下に本発明についてさらに詳細に説明する。
大気腐食環境中で錆が物理的に割れや空隙等の構造的欠
陥が少ないものであれば酸素や水さらに大気中の腐食性
物質の侵入を防ぐことにもなり、結果として大気腐食環
境を遮断し易く、また浮き錆や流れ錆の根本的な原因で
あるFeイオンの溶出を軽減する。
The present invention will be described in more detail below.
If the rust has few physical defects such as cracks and voids in the atmospheric corrosive environment, it will prevent the ingress of oxygen, water, and corrosive substances in the atmosphere, and as a result shut off the atmospheric corrosive environment. In addition, it reduces the elution of Fe ions, which is the fundamental cause of floating rust and flow rust.

【0013】本発明者らは鋼材表面を覆う錆を構成する
粒子の平均結晶粒径が一定の大きさ以下であれば、錆が
緻密になり高い防食機能を果たすことを知見した。平均
結晶粒径としては、具体的には 200nm以下であれば、
工業地帯や田園地帯はもとより、海塩粒子が飛来し最も
厳しい環境である海岸地帯においても錆の防食性は良好
である。
The present inventors have found that if the average crystal grain size of the particles forming the rust covering the surface of the steel material is not more than a certain size, the rust becomes dense and has a high anticorrosion function. If the average crystal grain size is specifically 200 nm or less,
The corrosion resistance of rust is good not only in industrial areas and rural areas but also in coastal areas where sea salt particles fly in and are the most severe environment.

【0014】なかでも、鋼表面が通常の大気腐食環境中
で安定な最終腐食生成物であるα−FeOOH で覆われてい
る場合、その鋼の耐候性がさらに良好となることを見出
した。このことは、α−FeOOH は熱力学的に安定であ
り、錆の相変態や溶解に伴う電気化学反応が抑制される
ためであると考えられる。
In particular, it has been found that when the steel surface is covered with α-FeOOH, which is a final corrosion product that is stable in a normal atmospheric corrosion environment, the weather resistance of the steel is further improved. It is considered that this is because α-FeOOH is thermodynamically stable and suppresses the electrochemical reaction associated with the phase transformation and dissolution of rust.

【0015】ただし、本発明で言う鋼とはステンレス鋼
やNi基合金等、通常沈澱型皮膜であるいわゆる錆を生成
しないものは含まず、主として耐候性鋼等の低合金鋼や
炭素鋼を指す。
However, the steel referred to in the present invention does not include stainless steel, Ni-based alloys and the like, which do not form so-called rust which is usually a precipitation type film, and mainly refers to low alloy steel such as weathering steel and carbon steel. .

【0016】また、本発明で言う錆とは、特にその構成
物質名を指定しない限り、一般の鉄の大気腐食により生
成するα−FeOOH 、γ−FeOOH 、Fe3O4 等の混在した腐
食生成物を指す。
The term "rust" as used in the present invention means that, unless the names of its constituents are specified, the corrosion produced by the atmospheric corrosion of general iron is a mixture of α-FeOOH, γ-FeOOH, Fe 3 O 4 and the like. Refers to something.

【0017】[0017]

【実施例】次に本発明の効果を実施例により明らかにす
る。実施例に用いた試験鋼の化学成分を表1に示す。鋼
表面を平均結晶粒径 200nm以下の錆層で覆うために
は、例えば特開平3 −320646号に示した方法により適当
濃度の硫酸クロム(III )水溶液を適当量塗布しながら
大気暴露を行えばよく、また 200nm以下のα−FeOOH
を覆うためには例えば特願平4 −199701号に示した方法
により適当濃度硫酸クロム(III )水溶液と適当濃度の
水酸化ナトリウム水溶液を適当量塗布しながら大気暴露
を行えばよい。また、塗布する水溶液の濃度を制御する
ことにより、錆の平均結晶粒径の制御は可能である。
EXAMPLES Next, the effects of the present invention will be clarified by examples. Table 1 shows the chemical composition of the test steel used in the examples. In order to cover the steel surface with a rust layer having an average crystal grain size of 200 nm or less, for example, by the method disclosed in JP-A-3-320646, an appropriate amount of an aqueous chromium (III) sulfate solution is applied while being exposed to the atmosphere. Well, α-FeOOH less than 200nm
In order to cover the above, for example, by the method described in Japanese Patent Application No. 4-199701, an appropriate concentration of chromium (III) sulfate aqueous solution and an appropriate concentration of sodium hydroxide aqueous solution are applied and exposed to the atmosphere. Further, the average crystal grain size of rust can be controlled by controlling the concentration of the applied aqueous solution.

【0018】試験は、0.05〜40mass. %の硫酸クロム
(III )水溶液を一週間に一回鋼面に塗布しながら3ケ
月間大気暴露を行い、あるいは上記処理の後、pH9の水
酸化ナトリウム水溶液を一週間に一回鋼面に塗布しなが
らさらに1ケ月間大気暴露を行うことにより、種々の平
均結晶粒径の錆あるいは種々の平均結晶粒径のα−FeOO
H で構成された錆で覆われた暴露試験片を作製し行っ
た。
The test was carried out by exposing the steel surface to a 0.05 to 40 mass.% Aqueous solution of chromium (III) sulfate once a week for 3 months while exposing it to the atmosphere, or after the above treatment, an aqueous sodium hydroxide solution of pH 9 was used. Was applied to the steel surface once a week and was exposed to the atmosphere for another month to obtain rust with various average grain sizes or α-FeOO with various average grain sizes.
An exposure test piece composed of H 2 and covered with rust was prepared and performed.

【0019】カッターナイフで錆層を鋼面が確認できる
まで約100mg 採取し粉砕して粉末試料とし、これを用い
て透過型電子顕微鏡法により錆の平均結晶粒径を測定し
た。
About 100 mg of the rust layer was collected with a cutter knife until a steel surface could be confirmed and pulverized into a powder sample, which was used to measure the average crystal grain size of rust by transmission electron microscopy.

【0020】この際、構成鉄化合物の同定は電子線回析
パターンをとることにより行った。
At this time, the constituent iron compounds were identified by taking an electron beam diffraction pattern.

【0021】試験片の寸法は150 ×60×3mm3とし、処理
前の表面はエメリー紙研磨およびバフ研磨を施し、鏡面
としておいたものを使用した。
The test piece had a size of 150 × 60 × 3 mm 3, and the surface before treatment was polished with emery paper and buffed and used as a mirror surface.

【0022】各試験片を同一条件のもとに、海岸地帯で
ある北九州市に10年間暴露した。
Each test piece was exposed to the coastal area of Kitakyushu for 10 years under the same conditions.

【0023】暴露期間中の平均の腐食速度(単位時間あ
たりの板厚減少量)を鋼板の重量を測定することにより
評価した。なお、暴露した試験片直下にはコンクリート
板を配置し、コンクリートの汚れの程度より、流れ錆量
を評価した。結果を表2、表3、図1および図2に示
す。
The average corrosion rate (amount of reduction in plate thickness per unit time) during the exposure period was evaluated by measuring the weight of the steel plate. A concrete plate was placed directly below the exposed test piece, and the amount of flow rust was evaluated based on the degree of dirt on the concrete. The results are shown in Tables 2 and 3 and FIGS. 1 and 2.

【0024】[0024]

【表1】 [Table 1]

【0025】[0025]

【表2】 [Table 2]

【0026】[0026]

【表3】 [Table 3]

【0027】図1に錆層の平均結晶粒径と腐食速度の関
係を示す。錆の平均結晶粒径が200nm以下であると腐
食速度は低下しており、錆が緻密で防食性の高いものと
なっていることが明らかである。さらに、図2に示すよ
うに錆層がα−FeOOH で構成されている場合、平均結晶
粒径が 200nm以下であれば防食性は特に大きいことが
判る。
FIG. 1 shows the relationship between the average crystal grain size of the rust layer and the corrosion rate. When the average crystal grain size of rust is 200 nm or less, the corrosion rate is low, and it is clear that the rust is dense and has high anticorrosion properties. Further, as shown in FIG. 2, when the rust layer is composed of α-FeOOH, it can be seen that the corrosion resistance is particularly large when the average crystal grain size is 200 nm or less.

【0028】また表2および表3に示すように、平均結
晶粒径が 200nmを超えると腐食速度が急激に上昇する
と共に、流れ錆量が特に増加する。逆に、 200nm以下
であると、ほとんど流れ錆が認められなかった。
Further, as shown in Tables 2 and 3, when the average crystal grain size exceeds 200 nm, the corrosion rate rapidly increases and the amount of flow rust increases particularly. On the contrary, when the thickness is 200 nm or less, almost no flow rust was observed.

【0029】[0029]

【発明の効果】本発明は、鋼材表面が平均結晶粒径 200
nm以下の錆層で覆われていることあるいは鋼材表面が
平均結晶粒径 200nm以下のα−FeOOH で覆われている
ことにより、大気腐食環境中で赤錆や黄錆等の浮き錆や
流れ錆をほとんど生じることない防食性の高い錆を有す
る鋼材が提供される。したがって、建築物や構造物など
の社会資本の充実に寄与するところが大きい。
According to the present invention, the surface of the steel material has an average crystal grain size of 200
Due to the fact that it is covered with a rust layer with a thickness of nm or less or the surface of the steel material is covered with α-FeOOH with an average crystal grain size of 200 nm or less, floating rust and flow rust such as red rust and yellow rust in the atmospheric corrosive environment A steel material having rust with high corrosion resistance that hardly occurs is provided. Therefore, it greatly contributes to the enhancement of social capital such as buildings and structures.

【図面の簡単な説明】[Brief description of drawings]

【図1】鋼板の腐食速度と表面錆の平均結晶粒径の関係
を示すグラフである。
FIG. 1 is a graph showing the relationship between the corrosion rate of a steel sheet and the average crystal grain size of surface rust.

【図2】鋼板の腐食速度とα−FeOOH で構成される表面
錆の平均結晶粒径の関係を示すグラフである。
FIG. 2 is a graph showing the relationship between the corrosion rate of a steel sheet and the average crystal grain size of surface rust composed of α-FeOOH.

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】鋼材表面が平均結晶粒径 200nm以下の錆
層で覆われていることを特徴とする耐候性に優れた鋼材
1. A steel material having excellent weather resistance, characterized in that the surface of the steel material is covered with a rust layer having an average crystal grain size of 200 nm or less.
【請求項2】鋼材表面が平均結晶粒径 200nm以下のα
−FeOOH で覆われていることを特徴とする耐候性に優れ
た鋼材。
2. A steel material having an average crystal grain size of 200 nm or less α
-A steel material with excellent weather resistance, which is characterized by being covered with FeOOH.
JP5248693A 1993-03-12 1993-03-12 Steel material with excellent weather resistance Expired - Lifetime JP2765425B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP5248693A JP2765425B2 (en) 1993-03-12 1993-03-12 Steel material with excellent weather resistance

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP5248693A JP2765425B2 (en) 1993-03-12 1993-03-12 Steel material with excellent weather resistance

Publications (2)

Publication Number Publication Date
JPH06264256A true JPH06264256A (en) 1994-09-20
JP2765425B2 JP2765425B2 (en) 1998-06-18

Family

ID=12916050

Family Applications (1)

Application Number Title Priority Date Filing Date
JP5248693A Expired - Lifetime JP2765425B2 (en) 1993-03-12 1993-03-12 Steel material with excellent weather resistance

Country Status (1)

Country Link
JP (1) JP2765425B2 (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5545264A (en) * 1994-04-26 1996-08-13 Eiwa Co., Ltd. Method of and apparatus for processing metal material
US6068712A (en) * 1998-01-08 2000-05-30 Kawasaki Steel Corporation Steel products having superior weathering, method of producing the steel products, and method of forming weathering protective rust on steel product surfaces
US6218027B1 (en) 1999-02-25 2001-04-17 Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd) Steel material excellent in corrosion resistance and fabric using the same
US7037388B2 (en) 1998-09-30 2006-05-02 Kobe Steel, Ltd. Steel plate for paint use and manufacturing method thereof
CN102925884A (en) * 2012-11-29 2013-02-13 北京科技大学 Hydrojet pretreatment method for accelerating stabilization of rust layer on surface of weathering resistant steel
CN105112623A (en) * 2015-07-10 2015-12-02 国网山东省电力公司电力科学研究院 Rapid stabilization method for weathering resistant steel

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5545264A (en) * 1994-04-26 1996-08-13 Eiwa Co., Ltd. Method of and apparatus for processing metal material
US6068712A (en) * 1998-01-08 2000-05-30 Kawasaki Steel Corporation Steel products having superior weathering, method of producing the steel products, and method of forming weathering protective rust on steel product surfaces
US7037388B2 (en) 1998-09-30 2006-05-02 Kobe Steel, Ltd. Steel plate for paint use and manufacturing method thereof
US6218027B1 (en) 1999-02-25 2001-04-17 Kabushiki Kaisha Kobe Seiko Sho (Kobe Steel, Ltd) Steel material excellent in corrosion resistance and fabric using the same
CN102925884A (en) * 2012-11-29 2013-02-13 北京科技大学 Hydrojet pretreatment method for accelerating stabilization of rust layer on surface of weathering resistant steel
CN105112623A (en) * 2015-07-10 2015-12-02 国网山东省电力公司电力科学研究院 Rapid stabilization method for weathering resistant steel

Also Published As

Publication number Publication date
JP2765425B2 (en) 1998-06-18

Similar Documents

Publication Publication Date Title
Ilevbare et al. Oxygen reduction reaction kinetics on chromate conversion coated Al-Cu, Al-Cu-Mg, and Al-Cu-Mn-Fe intermetallic compounds
JP5849868B2 (en) Steel material with excellent corrosion resistance
JP2010248567A (en) Surface-treated steel material excellent in corrosion resistance
Kim et al. Effects of Alloying Elements (Cr, Mn) on Corrosion Properties of the High‐Strength Steel in 3.5% NaCl Solution
JP3345023B2 (en) Surface treatment agent for steel and surface treated steel
JP2765425B2 (en) Steel material with excellent weather resistance
JP5942532B2 (en) Steel material with excellent corrosion resistance
JP2827878B2 (en) Surface treatment method for steel with excellent weather resistance
JP2884941B2 (en) Steel material excellent in weather resistance and method of forming rust layer
JP4455712B2 (en) Coated steel with atmospheric corrosion resistance
JPH0874070A (en) Concrete reinforcing bar excellent in corrosion resistance
JP2768173B2 (en) High weather resistant steel
JP2699733B2 (en) Method for promoting rust stabilization of steel
JP3367437B2 (en) Method to generate uniform weathering stable rust early
JP3668009B2 (en) Method for promoting rust stabilization of steel
JP3932779B2 (en) Surface-treated steel and coating film forming method
JP3972806B2 (en) Surface-treated steel with excellent salt resistance
JP2000054158A (en) Steel excellent in seashore weatherability
JP3219003B2 (en) Surface treatment agent for steel and surface treated steel
JP3267238B2 (en) Method to generate uniform weathering stable rust early
JP2827781B2 (en) Surface treatment method for steel
JPH11217676A (en) Surface treating agent for steel and surface treated steel
JPH06241982A (en) Method for evaluating stabilization of rust of weather resistant steel material
JP3416874B2 (en) Surface treatment method for highly designed steel
JP3307321B2 (en) Coated steel with excellent weather resistance

Legal Events

Date Code Title Description
FPAY Renewal fee payment (prs date is renewal date of database)

Free format text: PAYMENT UNTIL: 20080403

Year of fee payment: 10

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

Free format text: PAYMENT UNTIL: 20090403

Year of fee payment: 11

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

Free format text: PAYMENT UNTIL: 20100403

Year of fee payment: 12

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

Free format text: PAYMENT UNTIL: 20100403

Year of fee payment: 12

S111 Request for change of ownership or part of ownership

Free format text: JAPANESE INTERMEDIATE CODE: R313114

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

Year of fee payment: 12

Free format text: PAYMENT UNTIL: 20100403

R350 Written notification of registration of transfer

Free format text: JAPANESE INTERMEDIATE CODE: R350

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

Free format text: PAYMENT UNTIL: 20110403

Year of fee payment: 13

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

Free format text: PAYMENT UNTIL: 20120403

Year of fee payment: 14

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

Free format text: PAYMENT UNTIL: 20120403

Year of fee payment: 14

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

Free format text: PAYMENT UNTIL: 20130403

Year of fee payment: 15

EXPY Cancellation because of completion of term