JP3166352B2 - Implant components - Google Patents

Implant components

Info

Publication number
JP3166352B2
JP3166352B2 JP31514292A JP31514292A JP3166352B2 JP 3166352 B2 JP3166352 B2 JP 3166352B2 JP 31514292 A JP31514292 A JP 31514292A JP 31514292 A JP31514292 A JP 31514292A JP 3166352 B2 JP3166352 B2 JP 3166352B2
Authority
JP
Japan
Prior art keywords
implant member
pores
present
bioactive substance
living
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 - Lifetime
Application number
JP31514292A
Other languages
Japanese (ja)
Other versions
JPH06154257A (en
Inventor
洋司 川谷
隆夫 川井
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.)
Kobe Steel Ltd
Original Assignee
Kobe Steel 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
Application filed by Kobe Steel Ltd filed Critical Kobe Steel Ltd
Priority to JP31514292A priority Critical patent/JP3166352B2/en
Publication of JPH06154257A publication Critical patent/JPH06154257A/en
Application granted granted Critical
Publication of JP3166352B2 publication Critical patent/JP3166352B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Landscapes

  • Materials For Medical Uses (AREA)
  • Prostheses (AREA)

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【産業上の利用分野】本発明は人工骨,人工関節,人工
歯根等として使用される生体用インプラント部材に関
し、詳細には生体骨組織との固着力を強化する目的で表
面に適正な大きさの気孔が形成されると共に、この気孔
が形成した凹凸部が生体との適合性に優れた生体活性物
質で被覆されたインプラント部材に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an implant member for a living body used as an artificial bone, an artificial joint, an artificial tooth root, and the like. The present invention relates to an implant member in which pores are formed and an uneven portion formed by the pores is coated with a bioactive substance having excellent compatibility with a living body.

【0002】[0002]

【従来の技術】人工骨等の生体用インプラント部材に
は、生体組織との固着力を高める目的で表面に微細な凹
凸を形成することが行なわれている。この凹凸形成手段
の一例としては、基材表面に微細な粉粒体又は線状体を
付着する手段が挙げられ、粉粒体を付着するに当っては
プラズマ溶射法を利用し、プラズマの熱によって粉粒体
の表面を溶融し、これを基材表面へ衝突させて凹凸皮膜
を形成する。
2. Description of the Related Art In a living body implant member such as an artificial bone or the like, fine irregularities are formed on the surface for the purpose of increasing the adhesion force to a living tissue. As an example of the unevenness forming means, there is a means for adhering a fine powder or a granular material on the surface of the base material. As a result, the surface of the granular material is melted, and this is caused to collide with the surface of the base material to form an uneven film.

【0003】図2は従来のプラズマ溶射法によって凹凸
皮膜を形成したときのインプラント部材の気孔サイズの
発生頻度と気孔率の一例を示すものである。このグラフ
に示されるように最も多いのは気孔径が50μm以下の
極めて微小なものであり、新生生体組織の侵入及び固着
化に有利な100〜200μmのものは僅か2.1%程
度しかない。また全体の気孔率は合算しても37.3%
しかなく、生体組織との固着力は必らずしも高いレベル
になるものとは期待できない。
FIG. 2 shows an example of the frequency of occurrence of pore size and porosity of an implant member when a concavo-convex coating is formed by a conventional plasma spraying method. As shown in this graph, the largest number is extremely small with a pore diameter of 50 μm or less, and only about 2.1% has a pore diameter of 100 to 200 μm which is advantageous for invasion and fixation of a new living tissue. The total porosity is 37.3% in total
However, it cannot be expected that the adhesive force with the living tissue is necessarily at a high level.

【0004】[0004]

【発明が解決しようとする課題】そこで本発明者らは、
150〜350μmの気孔が多数存在して気孔率が高
く、しかも凹凸皮膜層における脱落発生の恐れが少ない
インプラント部材を提供すべく種々検討した結果、10
0〜400μmの粗粒子を基材表面へ付着することによ
り、基材表面に形成される凹凸皮膜に150〜350μ
mの大きさの気孔を高い比率で形成することができ、生
体組織の侵入及び固着を確実に行なえること、及びこの
凹凸皮膜を形成するに当たっては、10〜100μmの
微粒子をプラズマによって一部又は全部を溶融させるこ
とによって、上記粗粒子を付着させるための接着剤とし
て利用することができ、皮膜が外力によって脱落するの
を防止できることを見出し、先に特許出願を行なった
(特願平3−65640号)。
SUMMARY OF THE INVENTION Accordingly, the present inventors
As a result of various studies to provide an implant member having a large porosity with a large number of pores of 150 to 350 μm and a low risk of falling off of the uneven coating layer, 10
By adhering coarse particles of 0 to 400 μm to the surface of the base material, 150-350 μm
It is possible to form pores having a size of m at a high ratio, to ensure penetration and fixation of living tissue, and to form this uneven film, a part of fine particles of 10 to 100 μm are partially or It has been found that by melting the whole, it can be used as an adhesive for adhering the coarse particles, and that the film can be prevented from falling off by external force. No. 65640).

【0005】しかしながら、上記した方法で製造したイ
ンプラント部材そのものは、実際に人工骨等として生体
に埋植した場合生体適合性が充分ではなく、新生生体組
織の成長性に劣るという問題があった。
[0005] However, the implant member itself produced by the above-described method has a problem that when it is actually implanted in a living body as an artificial bone or the like, the biocompatibility is not sufficient, and the growth of a new living tissue is poor.

【0006】本発明は以上のような状況に鑑みてなされ
たものであって、その目的は、生体適合性に優れ、生体
埋植時の新生生体組織の侵入及び固着が確実に行なえる
インプラント部材を提供することにある。
The present invention has been made in view of the above circumstances, and an object of the present invention is to provide an implant member which is excellent in biocompatibility and can ensure penetration and fixation of a new living tissue at the time of implanting a living body. Is to provide.

【0007】[0007]

【課題を解決するための手段】上記課題を解決すること
のできた本発明のインプラント部材は、基材層表面に気
孔径150〜350μmの開口した気孔を多数含む凹凸
皮膜が形成され、かつ該気孔内面を生体活性物質によっ
て被覆するとともに該被覆量を2〜12mg/cm2
し、前記凹凸皮膜の剪断強度を200kgf/cm2
上とすることに要旨を有する。
According to the implant member of the present invention which can solve the above-mentioned problems, an irregular film containing a large number of open pores having a pore diameter of 150 to 350 μm is formed on the surface of a base material layer. The gist is that the inner surface is coated with a bioactive substance, the coating amount is 2 to 12 mg / cm 2, and the shear strength of the uneven film is 200 kgf / cm 2 or more.

【0008】[0008]

【作用】本発明のインプラント部材は、まず基材層表面
に気孔径が150〜350μmのものが多数を占める開
口した気孔部を有する凹凸皮膜を形成したものである。
即ち、気孔径が150〜350μmのものであれば、気
孔内面を後記のように生体活性物質で被覆しても気孔の
開口部が塞がれず、このため新生生体組織の侵入を容易
ならしめるとともに生体活性物質による被覆効果を十分
に発揮させることができる。
The implant member of the present invention is formed by first forming an uneven film having open pores occupying a large number of pores having a pore diameter of 150 to 350 μm on the surface of the substrate layer.
That is, if the pore diameter is 150 to 350 μm, even if the pore inner surface is coated with a bioactive substance as described below, the pore opening is not closed, thereby facilitating penetration of the new living tissue. The coating effect by the bioactive substance can be sufficiently exhibited.

【0009】本発明において上記気孔の内面を被覆する
生体活性物質の被覆量は2〜12mg/cm2 である必要が
ある。被覆量が2mg/cm2 未満であると生体活性物質に
よる生体適合性の向上効果が不十分で生体埋込み時に新
生骨の成長が不足する。一方12mg/cm2 を超えると気
孔内部の生体活性物質が多くなり過ぎてこれが気孔を埋
め、界面が平滑になるので気孔と生体組織との物理的結
合、即ちアンカー効果が消失して充分な固着と強度が得
られなくなる。
In the present invention, the coating amount of the bioactive substance covering the inner surface of the pores needs to be 2 to 12 mg / cm 2 . If the coating amount is less than 2 mg / cm 2 , the effect of improving the biocompatibility with the bioactive substance is insufficient, and the growth of new bone at the time of implanting the living body is insufficient. On the other hand, if it exceeds 12 mg / cm 2 , the amount of bioactive substance inside the pores becomes too large, which fills the pores and makes the interface smooth, so that the physical bonding between the pores and living tissue, ie, the anchor effect is lost and sufficient fixation occurs. And strength cannot be obtained.

【0010】本発明で用いる生体活性物質とは、生体親
和性が高く、部材表面において生体硬組織と化学結合を
生じるか、或いは生体硬組織に吸収置換されるものが好
ましく、バイオガラス,バイオ結晶化ガラス,ヒドロキ
シアパタイト,トリカルシウムフォスフェート等が例示
される。
The bioactive substance used in the present invention is preferably a substance having a high biocompatibility and capable of forming a chemical bond with living hard tissue on the surface of a member or being absorbed and replaced by living hard tissue. Examples include fossilized glass, hydroxyapatite, and tricalcium phosphate.

【0011】本発明においては、生体活性物質で被覆さ
れた気孔を有する凹凸皮膜の剪断強度は200kgf/cm2
以上とする。これは剪断強度が200kgf/cm2 未満の場
合、生体への埋植時に外力等によって凹凸皮膜の脱落が
生じて気孔部が消失してしまうので、その本来の効果で
ある生体組織との物理的結合性及び生体親和性が望めな
いからである。
In the present invention, the shear strength of the uneven film having pores coated with a bioactive substance is 200 kgf / cm 2.
Above. This is because when the shear strength is less than 200 kgf / cm 2, the pores are lost due to the fall of the uneven film due to external force and the like at the time of implantation in the living body, and the pores are lost. This is because binding and biocompatibility cannot be expected.

【0012】本発明のインプラント部材の製造方法は特
に限定されるものではないが、望ましくはプラズマ溶射
法によって粒径が100〜400μmの粉粒体を基材表
面に付着させるとともに、粒径が10〜100μmの微
粒子をプラズマによって溶融させて上記粗粒子を付着さ
せるための接着剤として利用して、粗粒子相互を結合さ
せ、その後この様にして形成された気孔の内面を生体活
性物質で被覆する方法が推奨される。尚この方法で本発
明のインプラント部材を形成するのに用いられる粉粒体
は、スポンジチタン粒,純チタン粒,チタン合金粒(好
ましくはα合金又はα+β合金)及びその他金属又はセ
ラミックスのいずれであってもよく、またインプラント
基材はTi,Ti合金はもとより、Zr,Zr合金,C
o−Cr−Mo合金、Co−Cr−W−Ni合金,T
a,ステンレス鋼等の金属材料が使用できる他、ヒドロ
キシアパタイトやアルミナ等のセラミックスも使用でき
る。
Although the method for producing the implant member of the present invention is not particularly limited, it is preferable that a powder having a particle diameter of 100 to 400 μm be adhered to the surface of the base material by a plasma spraying method, and that the particle diameter be 10 μm. Fine particles of about 100 μm are melted by plasma and used as an adhesive for adhering the coarse particles to bond the coarse particles to each other, and then the inner surface of the pores thus formed is coated with a bioactive substance. A method is recommended. The powder used to form the implant member of the present invention by this method may be any of sponge titanium particles, pure titanium particles, titanium alloy particles (preferably α alloy or α + β alloy), and other metals or ceramics. The implant substrate may be made of Zr, Zr alloy, C
o-Cr-Mo alloy, Co-Cr-W-Ni alloy, T
a, a metal material such as stainless steel can be used, and ceramics such as hydroxyapatite and alumina can also be used.

【0013】以下実施例を挙げて本発明を更に詳細に説
明するが、下記実施例は本発明を制限するものではな
く、前・後記の趣旨を逸脱しない範囲で変更実施するこ
とは全て本発明の技術的範囲に包含される。
Hereinafter, the present invention will be described in more detail with reference to examples. However, the following examples do not limit the present invention, and all changes and implementations without departing from the spirit of the present invention will be described. Within the technical scope of

【0014】[0014]

【実施例】【Example】

(1)2つのパウダーポートを有するプラズマガンを準
備し、1つのポートからは平均粒径350μmのスポン
ジチタン粗粒子を吐出し、他のポートからは粒径44μ
m以下のチタン微粒子を吐出した。そしてチタン合金製
のインプラント基材表面に向けて各ポートから交互にプ
ラズマ溶射を行ない、基材表面に150〜350μmの
気孔径サイズを有する凹凸皮膜を形成した。図1に形成
した皮膜の気孔径サイズ毎の発生頻度を示す。
(1) A plasma gun having two powder ports is prepared, and sponge titanium coarse particles having an average particle diameter of 350 μm are discharged from one port, and a particle diameter of 44 μm is discharged from another port.
m or less of titanium fine particles were discharged. Then, plasma spraying was performed alternately from each port toward the surface of the titanium alloy implant base material to form an uneven film having a pore size of 150 to 350 μm on the base material surface. FIG. 1 shows the frequency of occurrence for each pore size of the formed film.

【0015】尚該皮膜の厚さを1mm程度にするには、上
記微粒子と粗粒子の交互溶射を2〜8回繰り返せばよ
い。また、高い気孔率と強力な結合力を共に得るために
は、微粒子の溶射比率は5〜50%とすることが好まし
く、より好ましくは10〜40%とすることが推奨され
る。
In order to reduce the thickness of the coating to about 1 mm, the above-mentioned alternate spraying of fine particles and coarse particles may be repeated 2 to 8 times. In order to obtain both a high porosity and a strong bonding force, the spray ratio of the fine particles is preferably 5 to 50%, more preferably 10 to 40%.

【0016】(2)上記で形成した気孔部の全体の形状
を出すために調整加工した後熱処理し、引き続いて生体
活性物質としてバイオガラス(AWガラス)を表1に示
す被覆量で浸漬法によってコーティングした。その後結
晶化処理したものを被験動物(成犬)の股関節部に埋植
し、経時的に周辺組織とともに摘出して、新生骨組織の
成長度合いを評価した。表1に供試インプラント部材の
埋植前の皮膜の剪断強度と骨の成長度合いを示す。
(2) Heat treatment is performed after adjusting the shape of the pores formed above in order to obtain the entire shape thereof, and then bioglass (AW glass) as a bioactive substance is applied by a dipping method at a coating amount shown in Table 1. Coated. Thereafter, the crystallized one was implanted in the hip joint of a test animal (adult dog), extracted with the surrounding tissue over time, and the degree of growth of the new bone tissue was evaluated. Table 1 shows the shear strength of the coating and the degree of bone growth before implantation of the test implant member.

【0017】[0017]

【表1】 [Table 1]

【0018】表1から明らかなように本発明の規定要件
を満足する本発明材(No.1〜5)は埋植後の生体骨
の侵入・成長が速く、インプラント部材として優れてい
ることが分かる。比較材No.6は皮膜剪断強度は高い
が生体活性物質の被覆量が少ないために生体骨の侵入・
成長性に劣ることが分かる。比較材No.7は生体活性
物質の被覆量が過多であるので、前述の様に界面が平滑
になって生体組織との物理的結合が消失して充分な固着
と強度が得られない。よって、気孔部への新生骨の侵入
・成長が遅れる。また、埋植前の皮膜剪断強度が弱くな
っており、埋植の過程で外力によって凹凸皮膜が脱落
(剥離)してしまい所望の効果が得られなかった。
As is clear from Table 1, the materials of the present invention (Nos. 1 to 5) satisfying the requirements of the present invention have a high penetration and growth of living bone after implantation and are excellent as implant members. I understand. Comparative material No. No. 6 has a high film shear strength, but has a small amount of bioactive substance, so that the penetration of living bone
It can be seen that the growth is inferior. Comparative material No. In No. 7, since the coating amount of the bioactive substance is excessive, the interface becomes smooth as described above, and the physical bond with the living tissue is lost, so that sufficient fixation and strength cannot be obtained. Therefore, penetration and growth of the new bone into the stoma are delayed. In addition, the shear strength of the film before embedding was weakened, and the uneven film was dropped (peeled) by external force during the embedding process, and the desired effect could not be obtained.

【0019】尚本発明のインプラント部材の製造手段は
上記製造例に限定されるものではなく、粗粒子と微粒子
を同時にプラズマ溶射して、その後生体活性物質で被覆
しても、上記交互溶射によって製造されたインプラント
部材と同等の気孔径及び結合力を有するインプラント部
材を提供することができる。
The means for producing the implant member of the present invention is not limited to the above-mentioned production example. Even if the coarse particles and the fine particles are simultaneously plasma-sprayed and then coated with a bioactive substance, the method for producing the implant member by the above-mentioned alternate spraying can be used. It is possible to provide an implant member having the same pore diameter and bonding strength as the implant member that has been made.

【0020】[0020]

【発明の効果】本発明は以上の様に構成されており、生
体適合性に優れ、しかも手術時等における基材表面から
の凹凸皮膜の脱落が起こりにくく、新生生体組織の侵入
及び固着が確実に行えるインプラント部材を実現した。
また本発明のインプラント部材は、この様に皮膜の脱落
が防止できるので、脱落した粒子が関節摺動部等に侵入
して異常摩耗を引き起こすこともなくなり、人工股関節
等動きの多い部分へも適用できる。
Industrial Applicability The present invention is constituted as described above, is excellent in biocompatibility, hardly causes the uneven film to fall off from the surface of the base material at the time of operation or the like, and ensures penetration and fixation of the new living tissue. The implant member which can be performed is realized.
In addition, the implant member of the present invention can prevent the coating from falling off in this way, so that the dropped particles do not enter the sliding portions of the joint and cause abnormal wear, and can be applied to a portion having much movement such as an artificial hip joint. it can.

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

【図1】本発明のインプラント部材の凹凸皮膜における
気孔径サイズ毎の発生頻度の一例を示すグラフである。
FIG. 1 is a graph showing an example of the frequency of occurrence for each pore size in an uneven film of an implant member of the present invention.

【図2】従来のインプラント部材の凹凸皮膜における気
孔径サイズ毎の発生頻度の一例を示すグラフである。
FIG. 2 is a graph showing an example of a frequency of occurrence for each pore size in a concavo-convex coating of a conventional implant member.

───────────────────────────────────────────────────── フロントページの続き (58)調査した分野(Int.Cl.7,DB名) A61F 2/28 A61L 27/00 WPI(DIALOG)──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. 7 , DB name) A61F 2/28 A61L 27/00 WPI (DIALOG)

Claims (1)

(57)【特許請求の範囲】(57) [Claims] 【請求項1】 基材層表面に気孔径150〜350μm
の開口した気孔を多数含む凹凸皮膜が形成され、かつ該
気孔内面を生体活性物質によって被覆するとともに該被
覆量を2〜12mg/cm2 とし、前記凹凸皮膜の剪断
強度を200kgf/cm2 以上とすることを特徴とす
るインプラント部材。
1. A pore size of 150 to 350 μm on a surface of a base material layer.
And the inner surface of the pores is coated with a bioactive substance, the coating amount is 2 to 12 mg / cm 2, and the shear strength of the uneven film is 200 kgf / cm 2 or more. An implant member characterized in that:
JP31514292A 1992-11-25 1992-11-25 Implant components Expired - Lifetime JP3166352B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP31514292A JP3166352B2 (en) 1992-11-25 1992-11-25 Implant components

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP31514292A JP3166352B2 (en) 1992-11-25 1992-11-25 Implant components

Publications (2)

Publication Number Publication Date
JPH06154257A JPH06154257A (en) 1994-06-03
JP3166352B2 true JP3166352B2 (en) 2001-05-14

Family

ID=18061918

Family Applications (1)

Application Number Title Priority Date Filing Date
JP31514292A Expired - Lifetime JP3166352B2 (en) 1992-11-25 1992-11-25 Implant components

Country Status (1)

Country Link
JP (1) JP3166352B2 (en)

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB9821663D0 (en) * 1998-10-05 1998-11-25 Abonetics Ltd Foamed ceramics
JP4825955B2 (en) * 2003-06-13 2011-11-30 独立行政法人産業技術総合研究所 Biological implant material and method for producing the same
EP1864684B1 (en) * 2005-03-31 2013-05-08 Japan Science and Technology Agency Method for producing an artificial bone
JP5019346B2 (en) * 2005-12-12 2012-09-05 国立大学法人 岡山大学 Bone-compatible implant and method for producing the same
WO2019146012A1 (en) * 2018-01-24 2019-08-01 オリンパス株式会社 Bone prosthetic material and bone prosthetic material manufacturing method
CN109848407A (en) * 2019-04-12 2019-06-07 上海海事大学 Cobalt-chromium-tungsten alloy-coated tantalum carbide powder and preparation method thereof

Also Published As

Publication number Publication date
JPH06154257A (en) 1994-06-03

Similar Documents

Publication Publication Date Title
Swain et al. Effect of surface roughness on titanium medical implants
US4542539A (en) Surgical implant having a graded porous coating
JP4420816B2 (en) Metallic coating with apertures for joint replacement implants and method of manufacturing the same
Xuereb et al. Systematic review of current dental implant coating materials and novel coating techniques.
EP0760687B1 (en) A biomaterial and bone implant for bone repair and replacement
EP0560279B1 (en) Open cell tantalum structures for cancellous bone implants and cell and tissue receptors
EP2014319A1 (en) A bone tissue implant comprising strontium ions
JP2858126B2 (en) Biological implant material and its manufacturing method
JPS62503011A (en) Coating of buried body
US20050221259A1 (en) Dental or orthopaedic implant
JP2004358249A (en) Strontium-substituted apatite coating
US20030074081A1 (en) Non-uniform porosity tissue implant
EP1052949A1 (en) Hip joint socket
JPH0475013B2 (en)
US20180200062A1 (en) Implant and method for coating an implant main body
JP5069888B2 (en) Biological implant
JP3166352B2 (en) Implant components
US5482731A (en) Method for bonding a calcium phosphate coating to stainless steels and cobalt base alloys for bioactive fixation of artificial implants
JP2009514576A (en) Open-hole biocompatible surface layer for implants, method for production and use thereof
KR101822255B1 (en) A method for preparation of a metallic implant comprising biocompatable fluoride ceramic coating
JP2000210313A (en) Bone substitutive material having excellent bioaffinity
JPH072170B2 (en) Composite implant member and manufacturing method thereof
AU2002315469A1 (en) Prosthetic devices having diffusion-hardened surfaces and bioceramic coatings.
Kothari et al. Role of hydroxyapatite (HA) coatings in implants: A review
Niwa et al. Application of α-tricalcium phosphate coatings on titanium subperiosteal orthodontic implants reduces the time for absolute anchorage: a study using rabbit femora

Legal Events

Date Code Title Description
A01 Written decision to grant a patent or to grant a registration (utility model)

Free format text: JAPANESE INTERMEDIATE CODE: A01

Effective date: 20010206

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

Free format text: PAYMENT UNTIL: 20080309

Year of fee payment: 7

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

Free format text: PAYMENT UNTIL: 20090309

Year of fee payment: 8

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

Free format text: PAYMENT UNTIL: 20100309

Year of fee payment: 9

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

Free format text: PAYMENT UNTIL: 20100309

Year of fee payment: 9

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

Free format text: PAYMENT UNTIL: 20110309

Year of fee payment: 10

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

Free format text: PAYMENT UNTIL: 20110309

Year of fee payment: 10

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

Free format text: PAYMENT UNTIL: 20120309

Year of fee payment: 11

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

Free format text: PAYMENT UNTIL: 20120309

Year of fee payment: 11

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

Free format text: PAYMENT UNTIL: 20130309

Year of fee payment: 12

EXPY Cancellation because of completion of term
FPAY Renewal fee payment (event date is renewal date of database)

Free format text: PAYMENT UNTIL: 20130309

Year of fee payment: 12