中国组织工程研究 ›› 2022, Vol. 26 ›› Issue (16): 2526-2531.doi: 10.12307/2022.252

• 组织工程口腔材料 tissue-engineered oral materials • 上一篇    下一篇

不同气压热处理钯银合金与瓷结合的强度

渠  艳1,李洁银2,庄秀妹 3,叶剑涛3,叶秀华3   

  1. 1中山大学光华口腔医学院口腔医学研究所,广东省广州市  510000 ;2揭阳市人民医院口腔科,广东省揭阳市  522000;3中山大学孙逸仙纪念医院口腔科,广东省广州市  510120
  • 收稿日期:2021-06-11 修回日期:2021-06-16 接受日期:2021-07-22 出版日期:2022-06-08 发布日期:2021-12-22
  • 通讯作者: 叶秀华,硕士,医师,中山大学孙逸仙纪念医院口腔科,广东省广州市 510120
  • 作者简介:渠艳,女,1991年生,汉族,中山大学光华口腔医学院在读博士,主要从事口腔修复学研究。
  • 基金资助:
    国家自然科学基金青年科学基金项目(81600899),项目负责人:庄秀妹

Heating palladium-silver alloys under various reduced air pressures and ceramic bond strength

Qu Yan1, Li Jieyin2, Zhuang Xiumei3, Ye Jiantao3, Ye Xiuhua3   

  1. 1Institute of Stomatological Research, Guanghua School of Stomatology, Sun Yat-sen University, Guangzhou 510000, Guangdong Province, China; 2Department of Stomatology, Jieyang People’s Hospital, Jieyang 522000, Guangdong Province, China; 3Department of Stomatology, Sun Yat-sen Memorial Hospital, Sun Yat-sen University, Guangzhou 510120, Guangdong Province, China
  • Received:2021-06-11 Revised:2021-06-16 Accepted:2021-07-22 Online:2022-06-08 Published:2021-12-22
  • Contact: Ye Xiuhua, Master, Physician, Department of Stomatology, Sun Yat-sen Memorial Hospital, Sun Yat-sen University, Guangzhou 510120, Guangdong Province, China
  • About author:Qu Yan, Doctoral candidate, Institute of Stomatological Research, Guanghua School of Stomatology, Sun Yat-sen University, Guangzhou 510000, Guangdong Province, China
  • Supported by:
    the National Natural Science Foundation of China (Youth Program), No. 81600899 (to ZXM)

摘要:

文题释义:
扫描电镜:是介于透射电镜和光学显微镜之间的一种微观形貌观察手段,可直接利用样品表面材料的物质性能进行微观成像。扫描电镜的优点:①有较高的放大倍数,20-20万倍之间连续可调;②景深大,视野大,成像富有立体感,可直接观察各种试样凹凸不平表面的细微结构; 
内氧化:在合金的高温氧化过程中,除了形成表面氧化物以外,氧可能溶解并扩散进入合金内部,与合金中较活泼的组元发生反应而形成颗粒状氧化物沉积在合金内部的过程。相应的氧化物称内氧化物。只有当合金的组成和浓度满足一定条件时才会发生内氧化,纯金属则不会发生。

背景:不同气压热处理对钯银合金内氧化和金瓷结合强度的影响尚缺乏深入研究,且钯银合金的金瓷结合机制存在争议。
目的:评价不同气压热处理对钯银合金与瓷结合强度的影响。
方法:用失蜡铸造法制备钯银合金试件(尺寸:25 mm×3 mm×0.5 mm),随机分成7组,分别进行常压热处理(0.1 MPa)与减压热处理(氧分压分别为0.001 8,0.002 3,0.003 6,0.004 6,0.005 4,0.007 1 MPa),使用配有能谱仪的扫描电镜观察试件的显微形貌和合金元素成分。将经处理后的7组合金进行模拟的遮色瓷烧结程序,分析合金元素成分。制备钯银合金-瓷试件,扫描电镜观察试件的显微形貌,使用三点弯曲测试评价金瓷结合强度。
结果与结论:①扫描电镜显示,热处理合金表面出现小瘤状突起结构,随着热处理氧分压的增加,合金表面的小瘤数量迅速增多、体积增大;当氧分压升至0.007 1 MPa时,合金表面的小瘤相互融合连接成条索状或网状,最后几乎覆盖合金表面,与常压热处理合金表面小瘤覆盖情况相似。与热处理前相比,热处理后合金表面的氧化物含量明显增加,随着氧分压升高,合金表面氧化物含量呈减少趋势。②扫描电镜显示,各组金瓷界面显微结构相似,瓷与合金结合紧密,合金表层下可见条索状结构,随着氧分压升高,条索状结构增多,其渗透进金属的深度增大。模拟遮色瓷烧结后,合金表面的氧化物含量继续减少。③0.001 8,0.002 3,0.003 6 MPa组金瓷结合强度显著大于0.004 6,0.005 4,0.007 1,0.1 MPa组(P < 0.05),其余组间两两比较差异无显著性意义(P > 0.05)。④结果表明,上瓷前在较低的气压(≤0.003 6 MPa)下对钯银合金进行热处理能获得较高的金瓷结合强度,钯银合金的内氧化和表面氧化物含量与热处理气压关系密切。

https://orcid.org/0000-0002-8798-1619 (渠艳) 

中国组织工程研究杂志出版内容重点:生物材料;骨生物材料口腔生物材料纳米材料缓释材料材料相容性;组织工程

关键词: 材料, 钯银合金, 金瓷结合强度, 三点弯曲测试, 氧分压, 热处理, 扫描电镜, 内氧化

Abstract: BACKGROUND: The effect of heating under different reduced air pressures on the internal oxidation and metal-ceramic bond strength of palladium-silver alloys requires further research, and controversy exists with respect to the bonding mechanism between palladium-silver alloys and porcelain. 
OBJECTIVE: To assess the effect of heating under different reduced atmospheric pressure on the metal-ceramic bond strength of palladium-silver alloys.  
METHODS: Palladium-silver metallic specimens (25 mm× 3 mm× 0.5 mm) were prepared using a cast method. Specimens were randomly assigned to seven groups, and subjected to heat treatments under six different reduced air pressures of 0.001 8, 0.002 3, 0.003 6, 0.004 6, 0.005 4, and 0.007 1 MPa and under normal atmospheric pressure (0.1 MPa). Scanning electron microscopy and energy-dispersive spectroscopy were used to study the specimens’ microstructure and elemental composition. After treatment, alloys in the seven groups were subjected to a simulated opaque porcelain sintering procedure to analyze the alloying element composition. The palladium-silver alloy-ceramic specimens were prepared and the microscopic morphology of the specimens was observed with scanning electron microscope. The metal-ceramic bond strength was evaluated using a three-point bending test. 
RESULTS AND CONCLUSION: (1) Scanning electron microscope displayed that nodules-like protrusions appeared on the surface of the heat-treated alloy. As the oxygen partial pressure increased, the number and volume of nodules on the surface of the alloy increased rapidly. When the oxygen partial pressure increased to 0.007 1 MPa, the nodules on the surface of the alloy were fused and connected into a cord or mesh, and finally almost covered the surface of the alloy, which was similar to the coverage of nodules on the surface of the normal pressure heat treatment alloy. Compared with that before heat treatment, the oxide content on the alloy surface increased significantly after heat treatment. As the oxygen partial pressure increased, the oxide content on the alloy surface showed a decreasing trend. (2) Scanning electron microscopy showed that the microstructure of the metal-porcelain interface was similar in each group. The porcelain was tightly bonded to the alloy. The cord-like structure was visible under the surface of the alloy. As the oxygen partial pressure increased, the cord-like structure increased, and the depth of its penetration into the metal increased. After the simulated opaque porcelain was sintered, the oxide content on the alloy surface continued to decrease. (3) The group with heating under 0.001 8, 0.002 3, and 0.003 6 MPa had significantly higher bond strength than those of heating under 0.004 6, 0.005 4, 0.007 1 MPa, and 0.1 MPa groups (P < 0.05). No statistical differences were observed in the bond strengths between the other groups (P > 0.05). (4) The results show that heating palladium-silver alloys under a lower reduced air pressure (≤ 0.003 6 MPa) effectively improved its bonding strength with porcelain. The internal oxidation and the content of external oxides on the metal surface of palladium-silver alloys were closely related with air pressure in the heat treatment.

Key words: materials, Palladium-silver alloy, metal-ceramic bond strength, three-point bending test, oxygen partial pressure, heat treatment, scanning electron microscopy, internal oxidation

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