JP2984118B2 - Biological implant material and its manufacturing method - Google Patents
Biological implant material and its manufacturing methodInfo
- Publication number
- JP2984118B2 JP2984118B2 JP3315679A JP31567991A JP2984118B2 JP 2984118 B2 JP2984118 B2 JP 2984118B2 JP 3315679 A JP3315679 A JP 3315679A JP 31567991 A JP31567991 A JP 31567991A JP 2984118 B2 JP2984118 B2 JP 2984118B2
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- Japan
- Prior art keywords
- titanium
- porous layer
- spraying
- implant material
- bone
- Prior art date
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- Materials For Medical Uses (AREA)
- Dental Preparations (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は疾病、災害などにより、
骨機能や手足の関節機能が失われた場合にこれらを修復
するために用いられる整形外科用人工骨及び人工関節、
あるいは老齢、疾病などによって失われた歯牙を復元す
るために用いられる人工歯根等を構成する生体インプラ
ント材とその製法に関するものであり、更に詳しく述べ
ると、金属の基体にポーラス層を被着してなる生体イン
プラント材及びチタン又はチタン基合金からなる基体の
表面にチタンの窒化物や酸化物を被覆してなる生体イン
プラント材とその製法に関するものである。BACKGROUND OF THE INVENTION The present invention relates to diseases, disasters, etc.
Orthopedic artificial bones and artificial joints used to repair bone functions and joint functions of limbs when they are lost,
Or, it relates to a biological implant material constituting an artificial tooth root and the like used for restoring teeth lost due to aging, illness, and the like, and a method for producing the same. More specifically, a porous layer is applied to a metal substrate. The present invention relates to a biological implant material obtained by coating the surface of a substrate made of titanium or a titanium-based alloy with a nitride or oxide of titanium, and a method for producing the same.
【０００２】[0002]
【従来の技術】近年、インプラントロジ−の発展は目覚
ましいものがあり、人工心臓、人工血管、人工肺など様
々な人工臓器が医療の世界で活躍している。特に整形外
科の分野では、失われた関節機能を復元するための人工
関節が広く用いられ、また、歯科医療の分野では人工歯
根が脚光を浴びている。2. Description of the Related Art In recent years, the development of implantology has been remarkable, and various artificial organs such as artificial hearts, artificial blood vessels, and artificial lungs are playing an active part in the medical field. In particular, in the field of orthopedics, artificial joints for restoring lost joint functions are widely used, and in the field of dental medicine, artificial dental roots are in the spotlight.
【０００３】人工関節のうち、最も多用されている人工
股関節を例に取ると、その本格的な発展は６０年代のチ
ャンレ−型人工股関節に始まる。その後、毒性などの問
題から、手術時にボ−ンセメントを用いないセメントレ
ス人工股関節が開発された。[0003] Taking the most commonly used artificial hip joint as an example, its full-scale development begins with the Changle type artificial hip joint in the 1960s. Thereafter, cementless hip prostheses without using bone cement during surgery were developed due to problems such as toxicity.
【０００４】セメントレス人工股関節は、患者自身の骨
によってインプラントを固定しようとする考えによるも
のであり、骨内での固定力向上のため、インプラント表
面にビ−ズやメッシュによるポ−ラスコ−ティング処理
を施したものが開発され、８０年代後半には最盛期を迎
えた。[0004] The cementless hip prosthesis is based on the idea of fixing the implant with the patient's own bone. In order to improve the fixing force in the bone, the surface of the implant is porous-coated with beads or mesh. Processed versions were developed and reached their heyday in the late 1980s.
【０００５】インプラントの表面をポ−ラス化する技術
としては、上述のビ−ズコ−ト、メッシュコ−トの他
に、減圧プラズマ溶射やサンドブラスト処理、酸エッチ
ング処理などの方法がある。As a technique for making the surface of the implant porous, in addition to the above-described bead coating and mesh coating, there are methods such as low-pressure plasma spraying, sandblasting, and acid etching.
【０００６】また、チタンまたはチタン基合金からなる
基体の表面にチタンの酸化物や窒化物をＣＶＤ法、ＰＶ
Ｄ法、さらにプラズマＣＶＤ法、そしてイオン注入法等
を用いてコーティングしたものとして、特開昭６２−１
２２６６９号公報で説明される生体用インプラント部材
がある。In addition, titanium oxide or nitride is coated on the surface of a substrate made of titanium or a titanium-based alloy by a CVD method,
A method coated by a method D, a plasma CVD method, an ion implantation method, etc.
There is a living body implant member described in Japanese Patent No. 22669.
【０００７】[0007]
【従来技術の課題】上記の従来技術のうち、インプラン
トの表面をポーラス化するものには各方法共に一長一短
があるものの、以下のような問題点が共通してある。2. Description of the Related Art Among the above-mentioned prior arts, those for making the surface of an implant porous have advantages and disadvantages in each method, but have the following problems in common.
【０００８】金属イオン溶出量の増大 ポ−ラスコ−ティングにより表面積が増大することか
ら、金属イオンの溶出量が増大する。また金属チタンは
耐摩耗性に劣るため、術後短期間でのインプラントのマ
イクロム−ブメントにより、さらに金属イオンの溶出量
が増加する。これらの溶出金属イオンは、発ガン性が有
するばかりでなく、インプラントの固定性を低下させ、
抜去再手術を余儀なくする原因となる。Increase in metal ion elution amount Since the surface area is increased by the porous coating, the amount of metal ion elution increases. In addition, since titanium metal is inferior in wear resistance, the amount of metal ions eluted further increases due to the micro-movement of the implant in a short period after the operation. These eluted metal ions not only have carcinogenicity, but also reduce the fixation of the implant,
This may cause removal and reoperation.
【０００９】疲労強度の低下 インプラント材料は生体に利用されるので、十分な疲労
強度が必要とされるが、ビ−ズコ−トなどのポ−ラスコ
−トにおいては、疲労強度が６０〜７０％も低下するこ
とが知られている。疲労強度の低下は生体内でのインプ
ラントの破損を招く危険がある。[0009] Since the implant material is used for living organisms, sufficient fatigue strength is required. However, in the case of a porous coat such as bead coat, the fatigue strength is 60 to 70%. Is also known to decrease. The reduction in fatigue strength risks breaking the implant in vivo.
【００１０】粒子の脱落 一般にポ−ラス層はバルク材質に比べて脆いため、手術
時の打ち込みの際などにしばしば脱落を起こす。手術後
のインプラントの下面に数個の脱落粒子が認められる例
もある。これらの脱落粒子が摺動面に入り込んだ場合に
は、異常摩耗を引き起こし、人工関節は短期間でその機
能を失うことになる。Generally, the porous layer is more brittle than the bulk material, and thus often falls off at the time of driving during operation. In some cases, several dropped particles are observed on the lower surface of the implant after surgery. If these falling particles enter the sliding surface, they cause abnormal wear and the prosthesis loses its function in a short time.
【００１１】また、上記特許公報の生体用インプラント
はチタンの酸化物や窒化物よりなる緻密な表面層が平均
厚さ僅か０．１〜３０μm に被着してなるものであるが
表面層が薄く、緻密であるため骨の増殖生成が発生せ
ず、また強度、耐蝕性も十分なものではなかった。[0011] Further, the implant for living body of the above-mentioned patent publication has a dense surface layer made of titanium oxide or nitride applied to an average thickness of only 0.1 to 30 µm, but the surface layer is thin. Because of its high density, no bone growth was generated, and the strength and corrosion resistance were not sufficient.
【００１２】[0012]
【課題を解決するための手段】本発明は、上述の問題点
を解決すべく、チタンまたはチタン合金からなる基体の
少なくとも骨との接合面に酸素を０．８〜２．０ｗｔ
％、窒素を６．１〜９．６ｗｔ％を含む厚さ１００μm
〜３ｍｍのチタンを主要成分とするポ−ラス層を具備し
た生体インプラント材および、チタンまたはチタン合金
からなる基体の少なくとも骨との接合面に対してチタン
またはチタン合金を大気中、或いは大気と窒素ガスの混
合比が１：２〜２：１の雰囲気中または大気と酸素の混
合比が２：１〜４：１の雰囲気中にてアーク溶射法、フ
レーム溶射法、プラズマ溶射法或いはレーザー溶射法に
て溶射し厚さ１００μm 〜３ｍｍのチタンを主要成分と
するポーラス層を形成し、さらにこれを３００〜１６５
０℃の温度にて熱処理を行なうことを特徴とする生体イ
ンプラント材の製法を提供する。SUMMARY OF THE INVENTION In order to solve the above-mentioned problems, the present invention provides a substrate made of titanium or a titanium alloy containing at least 0.8 to 2.0 wt.
%, Containing 6.1 to 9.6 wt% nitrogen
A bioimplant material having a porous layer containing titanium as a main component and a titanium or titanium alloy in the air or nitrogen and the air at least on a joint surface of a base made of titanium or a titanium alloy with a bone; Arc spraying, flame spraying, plasma spraying, or laser spraying in an atmosphere having a gas mixture ratio of 1: 2 to 2: 1 or an atmosphere having an air and oxygen mixture ratio of 2: 1 to 4: 1. To form a porous layer having titanium as a main component and having a thickness of 100 μm to 3 mm.
A method for producing a biological implant material characterized by performing a heat treatment at a temperature of 0 ° C.
【００１３】[0013]
【実施例】以下、本発明を実施例により詳述する。図１
に示す如く、チタンまたはチタン合金の基体Ａ上に、大
気中或いは大気と窒素ガスまたは大気と酸素ガスを混合
した雰囲気中でア−ク溶射法などの方法でチタンまたは
チタン合金を溶射してポーラス層Ｂを形成し生体移植材
１を作製する。溶射法はフレ−ム溶射、プラズマ溶射及
びレ−ザ−溶射でも良いが、ア−ク溶射が最も粗いポ−
ラス面が得られる。なお、上記の溶射方法は単独でも、
２つ以上の方法を組合わせて用いても良い。なお、溶射
条件は、可及的に粗い面となるように選定されている。The present invention will be described below in detail with reference to examples. FIG.
The titanium or titanium alloy is sprayed onto the substrate A of titanium or titanium alloy by a method such as an arc spraying method in the air or in a mixed atmosphere of air and nitrogen gas or air and oxygen gas to form a porous material. The layer B is formed, and the living body transplant material 1 is manufactured. The thermal spraying method may be frame thermal spraying, plasma thermal spraying, or laser thermal spraying, but arc thermal spraying is the coarsest port.
A lath surface is obtained. In addition, even if the said spraying method is independent,
Two or more methods may be used in combination. Note that the thermal spraying conditions are selected so that the surface is as rough as possible.
【００１４】ポーラス層Ｂは、チタンまたはチタン合金
が上記雰囲気中酸素や窒素と反応し、酸化チタンや窒化
チタンを含みチタンを主要成分とするチタン組成物とな
っている。なお、このように形成したポーラス層Ｂにお
いて酸化チタン、窒化チタンの分布は表面部分に最も多
く集中する。特に表面には酸化チタンを主要成分とする
ミクロンオーダーの膜厚を有する被覆膜Ｂ1 が形成され
ているため、生体インプント１が耐蝕性に優れたものと
なっているとともに金属チタンの溶出が抑制され、また
ポーラス層Ｂ表面近傍に多く存在する窒化チタンによっ
て耐摩耗性にも優れ、またポーラス層Ｂ全体にわたって
存在している残りの窒化チタンによってポーラス層Ｂの
強度が強化され破壊が起こり難くなってており、更には
基体Ａとの接合強度も十分なものとなっている。なおこ
のように溶射中に化学反応を起こさせる反応溶射を用い
て形成したポーラス層Ｂを具備することが、本発明の生
体インプラント材１の最も大きな特長である。The porous layer B is a titanium composition containing titanium oxide and titanium nitride, in which titanium or a titanium alloy reacts with oxygen or nitrogen in the above atmosphere and contains titanium as a main component. In the porous layer B thus formed, the distribution of titanium oxide and titanium nitride is most concentrated on the surface portion. Especially since the coating film B 1 having a thickness of micron order to be a major component of titanium oxide is formed on the surface, dissolution of the metal titanium with the biological Inpunto 1 becomes excellent in corrosion resistance Suppressed, the titanium nitride present in the vicinity of the surface of the porous layer B has excellent wear resistance, and the remaining titanium nitride existing over the entire porous layer B enhances the strength of the porous layer B, so that the titanium layer hardly breaks. Further, the bonding strength with the base A is also sufficient. It is to be noted that the provision of the porous layer B formed by using the reaction spray for causing a chemical reaction during the spraying is the most significant feature of the biological implant material 1 of the present invention.
【００１５】上記ポーラス層Ｂは溶射後に熱処理を施す
事によって、さらに特性を改善することができるので、
３００℃〜１６５０℃で熱処理を行う。熱処理は基体Ａ
の酸化を防止するため、真空中、または不活性ガス雰囲
気中で行われる。なお、上記熱処理温度については３０
０℃以下ではポーラス層Ｂの歪み取り効果が無く、一方
１６５０℃以上では基体Ａが溶解してしまうので不適当
である。なお、最も好ましい熱処理温度領域は８５０℃
〜１２５０℃である。また、ポーラス層Ｂの厚みとして
は、１００μm 〜３ｍｍの範囲が適当である。１００μ
m 以下では十分な骨の増殖生成が発生せず、またインプ
ラント材としての寸法制約上、３ｍｍを超す厚みのチタ
ン溶射層は不適当である。The properties of the porous layer B can be further improved by performing a heat treatment after thermal spraying.
The heat treatment is performed at 300C to 1650C. Heat treatment is for substrate A
Is performed in a vacuum or in an inert gas atmosphere in order to prevent oxidation of. The heat treatment temperature is 30
If the temperature is lower than 0 ° C., the effect of removing the strain of the porous layer B is not obtained. On the other hand, if the temperature is higher than 1650 ° C., the base A dissolves. The most preferred heat treatment temperature range is 850 ° C.
１２1250 ° C. The thickness of the porous layer B is suitably in the range of 100 μm to 3 mm. 100μ
When the diameter is less than m, sufficient bone growth is not generated, and a titanium sprayed layer having a thickness exceeding 3 mm is not suitable due to dimensional restrictions as an implant material.
【００１６】実施例１ 直径６ｍｍ、長さ２３ｍｍのチタン合金製円柱である基
体Ａの表面をサンドブラストによって粗面化した後、ア
ーク溶射法にて純チタンを溶射した。溶射は大気中また
は表１に示すような比率によって大気と窒素ガスを混合
した雰囲気中或いは大気と酸素ガス混合した雰囲気中で
行った後９５０℃にて真空熱処理を行い、それぞれの雰
囲気条件につき２個の円柱状試験体を作製した。なおチ
タンは反応性が高いため、多量の酸素ガスの添加は危険
であり添加の上限は２０％（大気：O 2 ガス＝４：１）
とした。なお、ポーラス層Ｂの厚みは０．３〜０．４ｍ
ｍであった。 Example 1 The surface of a substrate A, which was a titanium alloy cylinder having a diameter of 6 mm and a length of 23 mm, was roughened by sandblasting, and then pure titanium was sprayed by an arc spraying method. Thermal spraying is performed in the atmosphere or in an atmosphere in which air and nitrogen gas are mixed or in an atmosphere in which air and oxygen gas are mixed at a ratio as shown in Table 1, and then a vacuum heat treatment is performed at 950 ° C. A plurality of cylindrical test pieces were prepared. Since titanium has high reactivity, it is dangerous to add a large amount of oxygen gas, and the upper limit of addition is 20% (atmosphere: O 2 gas = 4: 1).
And In addition, the thickness of the porous layer B is 0.3 to 0.4 m.
m.
【００１７】[0017]
【表１】 [Table 1]
【００１８】これらの円柱状試験体のうち各雰囲気条件
によるものにつき各１個を用いチャンバー内で塩水を３
日間にわたって噴霧し、腐食の発生状態を目視で評価す
る塩水噴霧法によるの加速腐食試験を行い耐蝕性を評価
した。その際の評価基準としては、Ａ：腐食発生認めら
れず、Ｂ：一部分のみに腐食が認められる、Ｃ：ステン
レスと同等またはやや良好な腐食状態が認められる、
Ｄ：ステンレスより劣る腐食状態が認められる、以上の
４段階を用いた。その評価結果を表１に示す。[0018] Of these cylindrical test specimens, one specimen was used for each of the atmospheric conditions, and 3 specimens of salt water were used in the chamber.
Spraying was performed over a period of days, and an accelerated corrosion test was performed by a salt spray method for visually evaluating the state of occurrence of corrosion to evaluate corrosion resistance. As evaluation criteria at that time, A: no corrosion was observed, B: corrosion was observed only in a part, C: corrosion state equivalent to or slightly better than stainless steel was observed,
D: The above four stages in which a corrosion state inferior to stainless steel was observed were used. Table 1 shows the evaluation results.
【００１９】また、上記の円柱状試験体のうち各雰囲気
条件によるものつき各残りの１個について各試験体をボ
ーンセメントに固定して押し出し試験を行い、目視によ
って試験体のポーラス層Ｂがボーンセメントと付着した
ままで、ボーンセメント内に破壊専断がおこっている
か、またはポーラス層Ｂとボーンセメントとの界面が剥
離専断しているのかについて、すなわちボーラス層Ｂの
ボーンセメントに対する付着性についての評価をした。
その際の評価基準としては、Ａ：ポーラス層Ｂの剥離全
く認められず、Ｂ：ポーラス層Ｂのごく一部のみに剥離
が認められる、Ｃ：ポーラス層Ｂが全体にわたって剥離
した、以上の３段階を用い、その評価の結果を表１に示
す。生体インプラント１として用いるためには耐蝕性及
び付着性のの評価が両方ともＢ以上であることが必要と
される。表１よりボーラス層Ｂとして好ましい酸素含有
率は０．８〜２．８wt％、また好ましい窒素含有率は
６．１〜９．６wt％であることが判る。For the remaining one of the above-mentioned cylindrical specimens under the respective atmospheric conditions, each specimen was fixed to bone cement and subjected to an extrusion test, and the porous layer B of the specimen was visually inspected for the bone layer. Evaluation of whether the fracture cement in the bone cement remains adhered to the cement or whether the interface between the porous layer B and the bone cement is peeled exclusively, ie, the adhesion of the bolus layer B to the bone cement Did.
As the evaluation criteria at that time, A: no peeling of the porous layer B was observed at all, B: peeling was observed only in a very small portion of the porous layer B, and C: the porous layer B was entirely peeled. Using the steps, the results of the evaluation are shown in Table 1. In order to be used as the biological implant 1, it is necessary that both the evaluation of corrosion resistance and the evaluation of adhesion are B or more. From Table 1, it can be seen that the preferred oxygen content for the bolus layer B is 0.8-2.8 wt%, and the preferred nitrogen content is 6.1-9.6 wt%.
【００２０】実施例２ 直径６ｍｍ，長さ２３ｍｍのチタン合金製円柱体である
３個の基体Ａの表面をサンドブラストによって粗面化し
た後、大気中でア−ク溶射法を用いて純チタンを溶射し
た。溶射後、それぞれに６５０℃、８５０℃及び１２５
０℃にて真空熱処理を施し３個の試験体を得た。なお、
試験体の窒素含有率は７．０wt％、酸素含有率は２．０
wt％、またポーラス層Ｂの厚みは約３００μmであっ
た。 Example 2 After the surfaces of three substrates A, each of which is a titanium alloy cylinder having a diameter of 6 mm and a length of 23 mm, were roughened by sandblasting, pure titanium was formed in the atmosphere by arc spraying. Sprayed. After thermal spraying, 650 ° C, 850 ° C and 125
Vacuum heat treatment was performed at 0 ° C. to obtain three test pieces. In addition,
The nitrogen content of the test specimen was 7.0 wt% and the oxygen content was 2.0
wt%, and the thickness of the porous layer B was about 300 μm.
【００２１】これらの円柱状試験体を用いて電気化学的
腐食試験を行い、孔食電位を測定した。液は３７℃の温
度に維持した生理食塩水を用い、掃引速度は５ｍＶ／ｓ
ｅｃで行った。また、同じように円柱状をした溶射なし
のチタン合金製基体Ａについても比較のため測定を行っ
たが、両方の結果を表２に示す。Using these columnar specimens, an electrochemical corrosion test was performed to measure the pitting potential. The liquid used was physiological saline maintained at a temperature of 37 ° C., and the sweep speed was 5 mV / s.
ec. In addition, the same measurement was carried out for a columnar-shaped titanium alloy substrate A without thermal spraying for comparison, and both results are shown in Table 2.
【００２２】[0022]
【表２】 [Table 2]
【００２３】表２から基体Ａの孔食電位２．００Ｖに対
し、１２５０℃で熱処理を施した円柱状試験体では極め
て高い電位が得られ、耐蝕性が大きく改善されているこ
とがわかる。また、他の試験体についても十分な耐蝕性
が認められた。一方、上述の方法で純チタンを溶射し８
５０℃で熱処理を施した円柱状試験体と別途用意したチ
タン合金製の基体Ａをオ−トクレ−ブを用いたイオン溶
出試験を行ったところ、同等レベルのイオン溶出量しか
示さなかった。従来のビ−ズコ−トなどによるポ−ラス
コ−トでは、チタン合金製の基体Ａの１０倍以上のイオ
ン溶出がある事が知られており、この実験から本発明の
生体インプラント１が優れ耐蝕性を有していることが証
明された。From Table 2, it can be seen that, with respect to the pitting corrosion potential of the substrate A of 2.00 V, an extremely high potential was obtained in the columnar specimen heat-treated at 1250 ° C., and the corrosion resistance was greatly improved. Sufficient corrosion resistance was also observed for the other test pieces. On the other hand, pure titanium was sprayed by
An ion elution test using an autoclave was performed on a columnar test body that had been heat-treated at 50 ° C. and a separately prepared titanium alloy substrate A, and only an equivalent level of ion elution was shown. It is known that a conventional bead-coated porous coating has ion elution more than 10 times that of the base A made of titanium alloy. From this experiment, the biological implant 1 of the present invention is superior in corrosion resistance. It was proved to have the property.
【００２４】実施例３ 図２に示すような、直径１２ｍｍ，長さ９０ｍｍで、中
央部Ａ1 のみ直径８ｍｍに削った３個の亜鈴型試験用の
基体Ａ（チタン合金製）の中央部Ａ1 に、大気中でレー
ザー溶射法を用いて純チタンの溶射を行い、それぞれに
６５０℃、８５０℃及び１２５０℃で真空熱処理を行い
厚み約２ｍｍのポーラス層Ｂを具備する試験体を作製し
た。なお、試験体の窒素含有率は７．０wt％、酸素含有
率は２．０wt％、であった。[0024] as shown in Example 3 Fig. 2, the diameter 12 mm, a length of 90 mm, the central portion A of the central portion A 1 only base A for the three dumbbell test shaved diameter 8 mm (made of titanium alloy) First , pure titanium was sprayed in the air using a laser spraying method, and vacuum heat treatment was performed at 650 ° C., 850 ° C., and 1250 ° C., respectively, to produce a test piece having a porous layer B having a thickness of about 2 mm. In addition, the nitrogen content of the test body was 7.0 wt%, and the oxygen content was 2.0 wt%.
【００２５】これらの試験体に対し、回転曲げ疲労試験
を行い、そのＳ−Ｎカ−ブから疲労限を求めた。また比
較のため上記亜鈴型試験用の基体Ａのみの疲労試験も行
った。その結果を表３に示す。A rotational bending fatigue test was performed on these specimens, and the fatigue limit was determined from the SN curve. For comparison, a fatigue test was performed only on the base A for the dumbbell-type test. Table 3 shows the results.
【００２６】[0026]
【表３】 [Table 3]
【００２７】表３が示すように、本発明の方法によるポ
−ラスコ−ティングでも基体の疲労強度の低下は多少あ
る。しかしながら、従来のビ−ズコ−トやメッシュコ−
トの場合、１２００℃の熱処理によって約７０％もの疲
労強度の低下があったのに比較すると、低下率は６５０
℃、８５０℃の熱処理の場合、４５％、１２５０℃の熱
処理の場合でも５１％と大きく改善されている。この疲
労強度の改善は、インプラントの安全性を向上させるも
のであり極めて重要である。As shown in Table 3, even in the porous coating by the method of the present invention, the fatigue strength of the substrate is slightly reduced. However, conventional bead coat and mesh coat
In the case of heat treatment, the heat treatment at 1200 ° C. reduced the fatigue strength by as much as about 70%.
In the case of heat treatment at 850 ° C. and 45 ° C., the heat treatment at 1250 ° C. is greatly improved to 51%. This improvement in fatigue strength is very important because it improves implant safety.
【００２８】実施例４ 直径２４ｍｍ，厚み２ｍｍのチタン円板よりなる基体Ａ
に大気中でフレーム溶射法を用いてチタン合金溶射し続
いてそれらの試験体を６５０℃で熱処理し、表４に示す
ような層厚のポーラス層Ｂを具備する複数の試験体を作
製した。なお、試験体の窒素含有率は７．０wt％、酸素
含有率は２．０wt％、であった。 Example 4 Base A made of a titanium disk having a diameter of 24 mm and a thickness of 2 mm
Then, a titanium alloy was sprayed in the atmosphere using a flame spraying method, and then the test pieces were heat-treated at 650 ° C. to produce a plurality of test pieces having a porous layer B having a layer thickness as shown in Table 4. In addition, the nitrogen content of the test body was 7.0 wt%, and the oxygen content was 2.0 wt%.
【００２９】[0029]
【表４】 [Table 4]
【００３０】上述のようにチタンのフレーム溶射によっ
て形成され、熱処理されたポーラス層Ｂの面粗さを測定
した結果を表４に示す。Table 4 shows the measurement results of the surface roughness of the porous layer B formed by the flame spraying of titanium as described above and subjected to the heat treatment.
【００３１】表３から明らかなように、層厚が５０μm
の時の最大面粗さはＲｍａｘ＝２１．３７μm とＲｍａ
ｘ２５μm 以下であり骨の増殖生成を誘導するには不十
分であるが、１００μm では３１．３３と骨の増殖生成
を誘導することが可能である。また、膜厚が３００μm
の時には、平均中心線面粗さ（Ｒａ）１９．９μm 、最
大面粗さ（Ｒmax ）１５１．６μm と非常に理想的な値
を得た。また、この時の表面状態はは図３の表面ＳＥＭ
像に示すような粗面になっていた。As is clear from Table 3, the layer thickness is 50 μm.
The maximum surface roughness at the time of Rmax is Rmax = 21.37 μm and Rmax
x 25 μm or less, which is insufficient for inducing bone growth and production, but 100 μm can induce bone growth and production of 31.33. In addition, the film thickness is 300 μm
In this case, the average center line surface roughness (Ra) was 19.9 μm, and the maximum surface roughness (Rmax) was 151.6 μm, which were very ideal values. The surface condition at this time is shown in FIG.
The surface was rough as shown in the image.
【００３２】従来のビ−ズコ−トによるポ−ラスコ−ト
では、ポ−ラス層を構成するビ−ズの粒径が０．２５ｍ
ｍ〜１ｍｍもあったため、手術時に骨に引っかかり粒子
の脱落を起こしていた。しかしながら、本発明の生体イ
ンプラント１の微細なポ−ラス層Ｂではこのような引っ
かかりは発生せず、ポ−ラス層の脱落は発生しない。In the conventional bead-coated porous coating, the beads constituting the porous layer have a particle size of 0.25 m.
Since the diameter was between m and 1 mm, the particles caught on the bone during the operation, causing the particles to fall off. However, in the fine porous layer B of the living body implant 1 of the present invention, such catching does not occur, and the porous layer does not fall off.
【００３３】実験例（動物実験） 直径３ｍｍ，長さ５０ｍｍのチタン合金棒の基体Ａにチ
タン合金を大気中でアーク溶射を用いて溶射して後８５
０℃で熱処理し、厚さ３００μm 及び５００μm のポー
ラス層Ｂを具備する２つの試験体を作製し、さらにプラ
ズマ溶射法を用いて溶射して後８５０℃で熱処理し、厚
さ５０μm 及び１００μm のポーラス層Ｂを具備する２
つの試験体を作製した。続いてこれらの試験体をウサギ
の脛骨に埋入し、現在術後観察中であるが、５０μm の
ポーラス層Ｂのもの以外については骨の増生侵入による
と思われる良好な固定性が得られている事が確認されて
いる。 Experimental Example (Animal Experiment) Titanium alloy was sprayed on the base A of a titanium alloy rod having a diameter of 3 mm and a length of 50 mm in the atmosphere using arc spraying, and then 85 mm.
Two specimens each having a porous layer B having a thickness of 300 μm and 500 μm were formed by heat treatment at 0 ° C., and were further sprayed using a plasma spraying method, followed by heat treatment at 850 ° C. to form a porous body having a thickness of 50 μm and 100 μm. 2 with layer B
Three specimens were prepared. Subsequently, these specimens were implanted in the tibia of a rabbit, and currently under postoperative observation, except for those having a porous layer B having a thickness of 50 μm, good fixation was attained which is considered to be due to bone invasion. Has been confirmed.
【００３４】[0034]
【発明の効果】上述のように本発明の生体インプラント
材は適量の酸素及び窒素を含むチタン合金の溶射層を含
んでいるため、生体内でのイオン溶出も少なく、インプ
ラント材として十分な疲労強度を持ち、ポ−ラス層の脱
落も起こしにくく、骨の増生侵入による良好な固定が得
られる優れた生体材料をもたらすことができる。As described above, since the biological implant material of the present invention contains a sprayed layer of a titanium alloy containing appropriate amounts of oxygen and nitrogen, ion elution in a living body is small, and sufficient fatigue strength as an implant material is obtained. This makes it possible to provide an excellent biomaterial that has a good fixation due to increased penetration of bone and hardly causes the porous layer to fall off.
【図１】本発明の生体インプラント材の部分側面図であ
る。FIG. 1 is a partial side view of a biological implant material of the present invention.
【図２】本発明実施例による回転曲げ試験に用いた試験
用の基体の側面図。FIG. 2 is a side view of a test substrate used in a rotary bending test according to an embodiment of the present invention.
【図３】本発明の生体インプラント材のポーラス層表面
を示す表面ＳＥＭ像図である。FIG. 3 is a surface SEM image showing the surface of a porous layer of the biological implant material of the present invention.
Ａ ：基体 Ａ1 ：中央部 Ｂ ：ポーラス層 Ｂ1 ：皮膜層 １ ：生体インプラント材A: substrate A 1: central B: porous layer B 1: coating layer 1: an implant material
Claims (2)
少なくとも骨との接合面に、酸素を０．８〜２．８ｗｔ
％、窒素を６．１〜９．６ｗｔ％を含む厚さ１００μm
〜３ｍｍのチタンを主要成分とするポ−ラス層を具備し
た生体インプラント材。At least at least a bonding surface of a substrate made of titanium or a titanium alloy with a bone is supplied with oxygen in an amount of 0.8 to 2.8 wt%.
%, Containing 6.1 to 9.6 wt% nitrogen
A biological implant material having a porous layer containing titanium of up to 3 mm as a main component.
少なくとも骨との接合面に対してチタンまたはチタン合
金を大気中、或いは大気と窒素ガスの混合比が１：２〜
２：１の雰囲気中または大気と酸素の混合比が２：１〜
４：１の雰囲気中にてアーク溶射法、フレーム溶射法、
プラズマ溶射法或いはレーザー溶射法にて溶射し厚さ１
００μm 〜３ｍｍのチタンを主要成分とするポーラス層
を形成し、さらにこれを３００〜１６５０℃の温度にて
熱処理を行なうことを特徴とする生体インプラント材の
製法。2. The method according to claim 1, wherein the titanium or titanium alloy is in the air or at a mixture ratio of the air and the nitrogen gas of at least 1: 2 with respect to at least the joint surface of the substrate made of titanium or the titanium alloy with the bone.
In a 2: 1 atmosphere or a mixture ratio of air and oxygen of 2: 1 to 1
Arc spraying, flame spraying in a 4: 1 atmosphere,
Sprayed by plasma spraying or laser spraying, thickness 1
A method for producing a biological implant material, comprising forming a porous layer containing titanium of 00 μm to 3 mm as a main component, and further performing a heat treatment at a temperature of 300 to 1650 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3315679A JP2984118B2 (en) | 1991-11-29 | 1991-11-29 | Biological implant material and its manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3315679A JP2984118B2 (en) | 1991-11-29 | 1991-11-29 | Biological implant material and its manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05146504A JPH05146504A (en) | 1993-06-15 |
| JP2984118B2 true JP2984118B2 (en) | 1999-11-29 |
Family
ID=18068261
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3315679A Expired - Fee Related JP2984118B2 (en) | 1991-11-29 | 1991-11-29 | Biological implant material and its manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2984118B2 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20230051344A (en) * | 2021-10-08 | 2023-04-18 | 재단법인 포항산업과학연구원 | Porous titanium powder, and method for manufacturing of the same |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1996024392A1 (en) * | 1995-02-07 | 1996-08-15 | Fidia Advanced Biopolymers, S.R.L. | Process for the coating of objects with hyaluronic acid, derivatives thereof, and semisynthetic polymers |
| US6613432B2 (en) * | 1999-12-22 | 2003-09-02 | Biosurface Engineering Technologies, Inc. | Plasma-deposited coatings, devices and methods |
| KR101296591B1 (en) * | 2012-04-20 | 2013-08-14 | 오스템임플란트 주식회사 | Post treatment device for ha coating layer of dental implant surface |
| KR20140080882A (en) * | 2012-12-20 | 2014-07-01 | (주)오티스바이오텍 | Bioactive Implant and Manufacturing Method of The Same |
-
1991
- 1991-11-29 JP JP3315679A patent/JP2984118B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20230051344A (en) * | 2021-10-08 | 2023-04-18 | 재단법인 포항산업과학연구원 | Porous titanium powder, and method for manufacturing of the same |
| KR102562983B1 (en) | 2021-10-08 | 2023-08-03 | 재단법인 포항산업과학연구원 | Porous titanium powder, and method for manufacturing of the same |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05146504A (en) | 1993-06-15 |
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