Development of refractory metal carbides and nitrides for dental materials and their biocompatibility

牙科材料用难熔金属碳化物和氮化物的开发及其生物相容性

• 批准号: 10307049
• 负责人: WATARI Fumio
• 金额: $ 24.19万
• 依托单位: HOKKAIDO UNIVERSITY
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for Scientific Research (A).
• 财政年份: 1998
• 资助国家: 日本
• 起止时间: 1998 至 2000
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/grant/KAKENHI-PROJECT-10307049/
• 关键词: Titanium nitride; Implant; Functionally gradient materials; Titanium; Abrasion particles; Biobompatibility; Ultrasonic scaler; Surface treatment; 引っかき硬さ; ビッカース硬さ; 窒化処理; 元素マッピング; アパタイト; 原子間力顕微鏡; 高融点金属

(I) REFRACTORY METALS : Biocompatibility was evaluated for IVA (Ti, Zr, Hf), VA (V,Nb, Ta), VIIIA (Re) group metals and others (Cu, Ag, Fe, Ni, stainless) by implantation test in rat. Metal dissolved region was visualized by supersensitive elemental mapping using XSAM (X-ray Scanning Analytical Microscope). Biocompatibility of refractory metals except V was confirmed. (II) SURFACE-NITRIDED TI : (1) Physical properties/Golden colored surface nitride layer is composed of TiN+Ti2N (Thin Film X-ray diffraction) with 2μm thickness (SEM observation of cross section) and Vickers hardness 1300. This remarkably high hardness resulted in no scratches produced even if an ultrasonic scaler used in clinical operation is applied. Rotated tribological abrasion test with constant load using an ultrasonic scaler was done for evaluation of scratch/abrasion resistance. (2) Biocompatibility/Biocompatibility of TiN was concluded approximately equivalent to Ti from quantitative analysis of direct contact ra … More tio of new bone to implant material and amount of new bone formation in animal implantation test. (3) Dental implantation test/The implant with its abutment composed of TiN was evaluated by miniature dental implantation test using mandibular molar teeth of rat. (4) Neutrophils cytotoxicity test of Ti minute abrasion powders/Soft tissue embedded with Ti powders of 10 μm and 1μm size showed inflammatory reaction even after 24 weeks. Phagocytosis of Ti particles by macrophage and change of morphology of neutrophils were observed. Cytokine TNF α was detected only for the case of 1μm Ti, which shows that the cytotoxicity also arises from physical size effect. (III) RELATED DERIVATIVE RESEARCH : (1) Functionally graded implant/Part of hydroxyapatite (HAP) suffers decomposition during sintering process of Ti/HAP functionally graded materials, while HAP is conserved without decomposition through sintering process in Ti/(HAP+TiN) system. (2) Functionally graded composite resin/To suppress the excessive stress concentration by impulsive force on upper crown part, which causes fracture in root part of tooth, when the core post is applied in residual tooth root, functionally graded composite resin with UDMA matrix and gradually changing silica filler content (0-80%) was produced by laser lithography. Stress relaxation effect was confirmed by optoelastic method and simulation using finite element method. (IV) CONCLUSION : Biocompatibility and extremely high surface hardness suggests potential applications promising where abrasion resistance is essential, such as (1) abutment part of dental implant where epithelium is penetrated through and (2) sliding surface of joints in artificial bone. Less

(I)耐火金属：通过大鼠体内植入试验，评价了IVA（Ti、Zr、Hf）、VA（V、Nb、Ta）、VIIIA（Re）族金属和其他金属（Cu、Ag、Fe、Ni、不锈钢）的生物相容性。金属溶解区域通过使用XSAM（X射线扫描分析显微镜）的超灵敏元素映射可视化。除V外，难熔金属的生物相容性得到证实。(II)表面氮化TI：（1）物理性能/金色表面氮化层由TiN+ Ti 2N（薄膜X射线衍射）组成，厚度为2μm（截面的SEM观察），维氏硬度为1300。这种非常高的硬度使得即使使用临床手术中使用的超声洁牙器也不会产生划痕。使用超声波定标器进行具有恒定载荷的旋转摩擦磨损试验以评价耐刮擦/耐磨性。(2)根据直接接触率的定量分析，TiN的生物相容性/生物相容性与Ti大致等同 ...更多信息 动物植入试验中新骨与植入材料的比值和新骨形成量。(3)牙种植试验/使用大鼠下颌磨牙，通过微型牙种植试验评价种植体及其基台（由TiN组成）。(4)钛微粉的中性粒细胞毒性试验/即使在24周后，10 μm和1μm大小的钛粉包埋的软组织也显示出炎症反应。观察巨噬细胞对钛颗粒的吞噬作用及中性粒细胞形态学变化。细胞因子TNF α仅在1μm Ti的情况下检测到，这表明细胞毒性也来自物理尺寸效应。(III)相关衍生研究：（1）Ti/HAP功能梯度材料在烧结过程中，植入体/部分羟基磷灰石（HAP）发生分解，而Ti/（HAP+TiN）系统中，HAP在烧结过程中不发生分解而保存下来。(2)功能梯度复合树脂/为了抑制上冠部分因冲击力而产生的过度应力集中，从而导致牙根部分的断裂，当将核桩应用于剩余牙根时，通过激光光刻制备具有UDMA基质和逐渐变化的二氧化硅填料含量（0-80%）的功能梯度复合树脂。通过光弹性方法和有限元模拟证实了应力松弛效应。(IV)结论：生物相容性和极高的表面硬度表明，在耐磨性至关重要的地方，例如（1）上皮穿透的牙科植入物的基台部分和（2）人工骨中关节的滑动表面，有潜在的应用前景。少

项目成果

宮尾里香: "放電プラズマ法による傾斜機能型インプラントの試作と特性"粉体および粉末冶金. 47. 1239-1242 (2000)

Rika Miyao：“使用放电等离子体方法的功能梯度植入物的原型生产和性能”粉末和粉末冶金。 47. 1239-1242 (2000)

M.UO,F.WATARI,A.YOKOYAMA et al.: "Dissolution of nickel and tissue response observed by X-ray analytical microscopy"Biomaterials. 20(8). 747-755 (1999)

M.UO、F.WATARI、A.YOKOYAMA 等人：“通过 X 射线分析显微镜观察镍的溶解和组织反应”生物材料。

F.SASOH,A.YOKOYAMA,M.UO,F.WATARI et al.: "Study on the fabrication and biocompatibility of titanium/hydroxyapatite functionally graded implant"J.Dent,Res.77(IADR Abstracts). 77. 839 (1998)

F.SASOH、A.YOKOYAMA、M.UO、F.WATARI 等：“钛/羟基磷灰石功能分级植入物的制造和生物相容性研究”J.Dent，Res.77（IADR Abstracts）。

Hironobu MATSUNO: "Biocompatibility and osteogenesis of refractory metal implants, titanium, hafnium, niobium, tantalum and rhenium"Biomaterials. (in press). (2001)

Hironobu MATSUNO：“难熔金属植入物、钛、铪、铌、钽和铼的生物相容性和成骨”生物材料。

田村豊: "生体用インプラントとしての窒化チタンの基礎的特性評価"平成12年度日本金属学会・日本鉄鋼協会両北海道支部合同冬期講演大会概要集. 14 (2001)

Yutaka Tamura：“氮化钛作为生物植入物的基本性能评估”日本金属研究所和日本钢铁研究所北海道分会2000年联合冬季会议摘要14（2001）。