微弧氧化法制备不同浓度含锌涂层表面特征及抗菌性能的研究
|
摘要
目的用微弧氧化法在纯钛表面制备不同浓度含锌涂层,比较其表面形貌、元素分布及抗菌性能。方法实验共分5组,抛光后纯钛作为对照组(CP组),未添加锌为无锌组(N-Zn组),根据引入不同浓度锌分为低锌组(L-Zn组)、中锌组(M-Zn组)、高锌组(H-Zn组);扫描电镜及能谱仪观察各组涂层表面形貌、元素分布;贴膜法测定涂层对大肠杆菌和金黄色葡萄球菌的抑制效果。结果①扫描电镜观察:CP组表面无孔洞结构,成沟槽形,4组实验组表面出现空洞结构,呈火山口样,N-Zn组、L-Zn组组表面纳米孔直径200～300 nm,M-Zn组表面纳米孔直径100～200 nm,H-Zn组表面纳米孔直径50～100 nm;②能谱仪显示,与CP组、N-Zn组相比,L-Zn、M-Zn、H-Zn组涂层表面成功引入了锌元素,且原子比例依次增高,具有显著统计学差异(P<0.01);③贴膜法实验结果:各组间菌落数相比,具有显著统计学差异(P<0.01)。结论微弧氧化法制备的含锌涂层具有抗菌性能,抗菌性能随锌离子浓度升高而增强。
Objective To prepare zinc-containing coatings with different concentrations on pure titanium by micro-arc oxidation, and to compare the surface morphology, element distribution and antibacterial properties. Methods The experiment was divided into 5 groups. Pure titanium after polishing was used as the control group(Group CP), the one without added zinc was used as zinc-free group(Group N-Zn). According to the introduction of different concentrations, zinc was divided into low-zinc group(Group L-Zn), medium-zinc group(Group M-Zn) and high-zinc group(Group H-Zn). SEM and EDS were used to observe the surface morphology and element distribution of each group. Film coating method was used to test the inhibitory effect of the coating on Escherichia coli and Staphylococcus aureus. Results ①SEM observation:There was no pore structure on the surface of Group CP, and troughs were formed. The voids on the surface of the four experimental groups showed a crater-like structure. The diameter of the nanopore on the surface of group N-Zn and L-Zn was 200-300 nm, the diameter of the nanopore on the surface of group M-Zn was 100-200 nm, and the diameter of nanopore on the surface of group H-Zn was 50-100 nm. ②EDS showed that compared with Goup CP and Group N-Zn, zinc was successfully introduced on the surface of the coating in groups L-Zn,M-Zn and H-Zn, and the atomic ratio increased in turn, there was a significant statistical difference(P<0.01). ③Film coating test results:There was a statistically significant difference in the number of colonies between the groups(P<0.01). Conclusion The zinc-containing coating prepared by micro-arc oxidation has antibacterial properties, and the antibacterial property increases with the increase of zinc ion concentration.
Objective To prepare zinc-containing coatings with different concentrations on pure titanium by micro-arc oxidation, and to compare the surface morphology, element distribution and antibacterial properties. Methods The experiment was divided into 5 groups. Pure titanium after polishing was used as the control group(Group CP), the one without added zinc was used as zinc-free group(Group N-Zn). According to the introduction of different concentrations, zinc was divided into low-zinc group(Group L-Zn), medium-zinc group(Group M-Zn) and high-zinc group(Group H-Zn). SEM and EDS were used to observe the surface morphology and element distribution of each group. Film coating method was used to test the inhibitory effect of the coating on Escherichia coli and Staphylococcus aureus. Results ①SEM observation:There was no pore structure on the surface of Group CP, and troughs were formed. The voids on the surface of the four experimental groups showed a crater-like structure. The diameter of the nanopore on the surface of group N-Zn and L-Zn was 200-300 nm, the diameter of the nanopore on the surface of group M-Zn was 100-200 nm, and the diameter of nanopore on the surface of group H-Zn was 50-100 nm. ②EDS showed that compared with Goup CP and Group N-Zn, zinc was successfully introduced on the surface of the coating in groups L-Zn,M-Zn and H-Zn, and the atomic ratio increased in turn, there was a significant statistical difference(P<0.01). ③Film coating test results:There was a statistically significant difference in the number of colonies between the groups(P<0.01). Conclusion The zinc-containing coating prepared by micro-arc oxidation has antibacterial properties, and the antibacterial property increases with the increase of zinc ion concentration.
引文
[1] Zhao Y,Wong SM,Wong HM,et al.Effects of carbon and nitrogen plasma immersion ion implantation on in vitro and in vivo biocompatibility of titanium alloy[J].ACS Appl Mater Interfaces,2013,5(4):1510-1516.
[2] Huang J,Li X,Koller GP,et al.Electrohydrodynamic deposition of nanotitanium doped hydroxyapatite coating for medical and dental applications[J].J Mater Sci Mater Med,2011,22(3):491-496.
[3] 张晶,刘丽.微量元素修饰钛种植体表面方法的研究进展[J].口腔医学,2014,34(3):221-224.
[4] 丁明超,李德超.种植体表面制备载银涂层的方法[J].中国口腔种植学杂志,2011,16(2):139-143.
[5] Rokosz K,Hryniewicz T,Matysek D,et al.SEM,EDS and XPS analysis of the coatings obtained on titanium after plasma electrolytic oxidation in electrolytes containing copper nitrate[J].Materials,2016,9(5):318.
[6] Zhang JY,Ai HJ,Qi M.Osteoblast growth on the surface of porous Zn-containing HA/TiO2,hybrid coatings on Ti substrate byMAO plus sol-gel methods[J].Surf Coat Tech,2013,228(9):S202-S205.
[7] Huang Y,Zhang X,Mao H,et al.Osteoblastic cell responses and antibacterial efficacy of Cu/Zn co-substituted hydroxyapatite coatings on pure titanium using electro deposition method[J].Rsc Advances,2015,5(22):17076-17086.
[8] Zhao BH,Zhang W,Wang DN,et al.Effect of Zn content on cytoactivity and bacteriostasis of micro-arc oxidation coatings onpure titanium[J].Surf Coat Tech,2013,228(8):S428-S432.
[9] Norowski PA,Bumgardner JD.Biomaterial and antibiotic strategies for peri-implantitis:a review[J].J Biomed Mater Res B Appl Biomater,2010,88B (2):530-543.
[10] Wadhwani CPK,Raval NC,Ramer N.Peri-implant disease and cemented implant restorations:A multifactorial etiology[J].Compend Contin Educ Dent,2013,34(1):32.
[11] Zhao QM,Li GZ,Zhu HM,et al.Studyon Effects of titanium surface microporous coatings containing zinc on osteoblast adhesion and its antibacterial activity[J].Appl Bionics Biomech,2017,2017:1-4.
[12] Zhao Q,Cheng L,Liu Z,et al.Surfacecharacteristics of Zinc–TiO2 coatings prepared via micro-arc oxidation[J].Compos Interface,2014,21(6):585-593.
[13] Hu H,Zhang W,Qiao Y,et al.Antibacterial activity and increased bone marrow stem cell functions of Zn-incorporated TiO2 coatings on titanium[J].Acta Biomater,2012,8(2):904-915.
[14] 况慧娟,杨林,许恒毅,等.纳米氧化锌抗菌性能及机制的研究进展[J].中国药理学与毒理学杂志,2015,29(1):153-157.
[15] Madhumitha G,Elango G,Roopan SM.Biotechnological aspects of ZnO nanoparticles:overview on synthesis and its applications[J].Appl Microbiol Biotech,2015,100(2):571-581.
[16] 屈晓莉,常灿光.镁合金压铸模铸件微弧氧化表面处理工艺研究[J].铸造技术,2016(2):252-255.
[17] 杨清岭,赵欣,魏大庆,等.微弧氧化钛基体含Si、Ca涂层的表征及植入兔胫骨影像学和力学性能研究[J].口腔医学研究,2012,28(6):534-536.
[18] 冯娇,刘海蓉,李永生,等.纳米羟基磷灰石/聚酰胺6医用复合材料的制备及性能表征[J].复合材料学报,2015,32(6):1602-1610.
[19] 马春秀,刘继光,张慧明,等.纯钛阳极氧化-植酸-载铜膜层的细胞相容性与抗菌性研究[J].医学理论与实践,2018,31(10):1405-1408.
[20] Xu J,Ding G,Li J,et al.Zinc-ion implanted and deposited titanium surfaces reduce adhesion of Streptococccus mutans[J].Appl Surf Sci,2010,256(24):7540-7544.
[2] Huang J,Li X,Koller GP,et al.Electrohydrodynamic deposition of nanotitanium doped hydroxyapatite coating for medical and dental applications[J].J Mater Sci Mater Med,2011,22(3):491-496.
[3] 张晶,刘丽.微量元素修饰钛种植体表面方法的研究进展[J].口腔医学,2014,34(3):221-224.
[4] 丁明超,李德超.种植体表面制备载银涂层的方法[J].中国口腔种植学杂志,2011,16(2):139-143.
[5] Rokosz K,Hryniewicz T,Matysek D,et al.SEM,EDS and XPS analysis of the coatings obtained on titanium after plasma electrolytic oxidation in electrolytes containing copper nitrate[J].Materials,2016,9(5):318.
[6] Zhang JY,Ai HJ,Qi M.Osteoblast growth on the surface of porous Zn-containing HA/TiO2,hybrid coatings on Ti substrate byMAO plus sol-gel methods[J].Surf Coat Tech,2013,228(9):S202-S205.
[7] Huang Y,Zhang X,Mao H,et al.Osteoblastic cell responses and antibacterial efficacy of Cu/Zn co-substituted hydroxyapatite coatings on pure titanium using electro deposition method[J].Rsc Advances,2015,5(22):17076-17086.
[8] Zhao BH,Zhang W,Wang DN,et al.Effect of Zn content on cytoactivity and bacteriostasis of micro-arc oxidation coatings onpure titanium[J].Surf Coat Tech,2013,228(8):S428-S432.
[9] Norowski PA,Bumgardner JD.Biomaterial and antibiotic strategies for peri-implantitis:a review[J].J Biomed Mater Res B Appl Biomater,2010,88B (2):530-543.
[10] Wadhwani CPK,Raval NC,Ramer N.Peri-implant disease and cemented implant restorations:A multifactorial etiology[J].Compend Contin Educ Dent,2013,34(1):32.
[11] Zhao QM,Li GZ,Zhu HM,et al.Studyon Effects of titanium surface microporous coatings containing zinc on osteoblast adhesion and its antibacterial activity[J].Appl Bionics Biomech,2017,2017:1-4.
[12] Zhao Q,Cheng L,Liu Z,et al.Surfacecharacteristics of Zinc–TiO2 coatings prepared via micro-arc oxidation[J].Compos Interface,2014,21(6):585-593.
[13] Hu H,Zhang W,Qiao Y,et al.Antibacterial activity and increased bone marrow stem cell functions of Zn-incorporated TiO2 coatings on titanium[J].Acta Biomater,2012,8(2):904-915.
[14] 况慧娟,杨林,许恒毅,等.纳米氧化锌抗菌性能及机制的研究进展[J].中国药理学与毒理学杂志,2015,29(1):153-157.
[15] Madhumitha G,Elango G,Roopan SM.Biotechnological aspects of ZnO nanoparticles:overview on synthesis and its applications[J].Appl Microbiol Biotech,2015,100(2):571-581.
[16] 屈晓莉,常灿光.镁合金压铸模铸件微弧氧化表面处理工艺研究[J].铸造技术,2016(2):252-255.
[17] 杨清岭,赵欣,魏大庆,等.微弧氧化钛基体含Si、Ca涂层的表征及植入兔胫骨影像学和力学性能研究[J].口腔医学研究,2012,28(6):534-536.
[18] 冯娇,刘海蓉,李永生,等.纳米羟基磷灰石/聚酰胺6医用复合材料的制备及性能表征[J].复合材料学报,2015,32(6):1602-1610.
[19] 马春秀,刘继光,张慧明,等.纯钛阳极氧化-植酸-载铜膜层的细胞相容性与抗菌性研究[J].医学理论与实践,2018,31(10):1405-1408.
[20] Xu J,Ding G,Li J,et al.Zinc-ion implanted and deposited titanium surfaces reduce adhesion of Streptococccus mutans[J].Appl Surf Sci,2010,256(24):7540-7544.