不同化学处理方法对PEEK材料表面改性及生物学行为的影响
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摘要
目的:采用不同化学处理方法对PEEK材料进行表面改性,提高PEEK材料的生物性能。方法:根据不同的化学处理方法分为5组(n=9):①空白对照组(PEEK):PEEK材料表面机械抛光,不进行酸处理;②浓硫酸处理5 min组(S1-PEEK);③浓硫酸处理10 min组(S2-PEEK);④浓硫酸处理5 min后,硝酸处理5 min(S+n-PEEK);⑤高锰酸钾+磷酸处理PEEK(Mn-PEEK);处理后五组材料在100℃水浴加热4 h。FE-SEM观察样本表面形貌,XPS检测样本化学组成,SEM观察细胞在材料表面的状态。结果:①组样本表面光滑,②、③、④组样本表面可见3D筛状孔结构,⑤组样本表面形成花瓣样结构。①、②、③、④、⑤中硫元素的质量百分比分别为:0、2. 45±0. 22、3. 48±0. 16(与②组比较,P=0. 000)、1. 79±0. 05(与②组比较,P=0. 002)和0。各试验材料表面培养的BMSCs细胞及伪足数量均多于对照组。结论:酸蚀PEEK材料可增加其表面生物性能;水浴可去除材料表面残余酸,进一步提高PEEK材料表面的生物性能。
Objective: To improve the bioactivity of PEEK by chemical methods. Methods: PEEK samples were treated by polish only( group(1)); concentrated sulfuric acid for 5 min( group(2)); concentrated sulfuric acid for 10 min( group(3)); concentrated sulfuric acid for 5 min,followed by treatment of hydrogen nitrate for 5 min( group(4)) and mineral chameleon and ortho-phosphoric acid( group(5)) respectively( n = 9). Then,all samples were treated by water at 100 ℃ for 4 h. The sample surface was observed by FE-SEM,the chemical comporent of the samples was analyzed by XPS. BMSCs were cultured on the sample surface for 4 h and observed by SEM. Results: The sample sureface in group(1) was smooth,in group(2),(3) and(4) was with 3 D ethmoidal foramen structure,in group(5) with petal-like from. The sulfur content( Wt%) of the samples of group(1),(2),(3),(4) and(5) was 0,2. 45 ± 0. 22,3. 48 ± 0. 16( vs(1),P= 0. 000),1. 79 ± 0. 05( vs(1) P = 0. 002) and 0 respectively. BMSCs cultured on the sample surface of group(2),(3),(4) and(5) were more and with more pseudopod. Conclusion: The bioactivity of PEEK can be enhanced after acid pickling. Water bath and nitric acid treatment can remove the residual acid and further enhance the bioactivity of PEEK.
Objective: To improve the bioactivity of PEEK by chemical methods. Methods: PEEK samples were treated by polish only( group(1)); concentrated sulfuric acid for 5 min( group(2)); concentrated sulfuric acid for 10 min( group(3)); concentrated sulfuric acid for 5 min,followed by treatment of hydrogen nitrate for 5 min( group(4)) and mineral chameleon and ortho-phosphoric acid( group(5)) respectively( n = 9). Then,all samples were treated by water at 100 ℃ for 4 h. The sample surface was observed by FE-SEM,the chemical comporent of the samples was analyzed by XPS. BMSCs were cultured on the sample surface for 4 h and observed by SEM. Results: The sample sureface in group(1) was smooth,in group(2),(3) and(4) was with 3 D ethmoidal foramen structure,in group(5) with petal-like from. The sulfur content( Wt%) of the samples of group(1),(2),(3),(4) and(5) was 0,2. 45 ± 0. 22,3. 48 ± 0. 16( vs(1),P= 0. 000),1. 79 ± 0. 05( vs(1) P = 0. 002) and 0 respectively. BMSCs cultured on the sample surface of group(2),(3),(4) and(5) were more and with more pseudopod. Conclusion: The bioactivity of PEEK can be enhanced after acid pickling. Water bath and nitric acid treatment can remove the residual acid and further enhance the bioactivity of PEEK.
引文
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[3]Yan P,Xu D,Wang Y,et al.Effect of barium-containing glass filler reinforcement on shear bond strength of poly(ether ether ketone)to resin cement[J].High Perfor Pol,2013,25(4):475-481.
[4]Vander Sloten J,Labey L,Van Audekercke R,et al.Materials selection and design for orthopaedic implants with improved long-term performance[J].Biomaterials,1998,19(16):1455-1459.
[5]Williams D.New horizons for thermoplastic polymers[J].Med Dev Tech,2001,12(4):8-9.
[6]Wang L,He S,Wu X,et al.Polyetheretherketone/nanofluorohydroxyapatite composite with antimicrobial activity and osseointegration properties[J].Biomaterials,2014,35(25):6758-6775.
[7]Mahjoubi H,Buck E,Manimunda P,et al.Surface phosphonation enhances hydroxyapatite coating adhesion on polyetheretherketone and its osseointegration potential[J].Acta Biomater,2017,47:149-158.
[8]Shimizu T,Fujibayashi S,Yamaguchi S,et al.Bioactivity of sol-gel-derived Ti O2 coating on polyetheretherketone:In vitro and in vivo studies[J].Acta Biomater,2016,35:305-317.
[9]Wong KL,Wong CT,Liu WC,et al.Mechanical properties and in vitro response of strontium-containing hydroxyapatite/polyetheretherketone composites[J].Biomaterials,2009,30(23-24):3810-3817.
[10]Lu T,Wen J,Qian S,et al.Enhanced osteointegration on tantalum-implanted polyetheretherketone surface with bonelike elastic modulus[J].Biomaterials,2015,51:173-183.
[11]Ouyang L,Zhao Y,Jin G,et al.Influence of sulfur content on bone formation and antibacterial ability of sulfonated PEEK[J].Biomaterials,2016,83:115-126.
[12]Lu T,Qian S,Meng F,et al.Enhanced osteogenic activity of poly ether ether ketone using calcium plasma immersion ion implantation[J].Colloids Surf B Biointerfaces,2016,142:192-198.
[13]Devine DM,Hahn J,Richards RG,et al.Coating of carbon fiber-reinforced polyetheretherketone implants with titanium to improve bone apposition[J].J Biomed Mater Res B Appl Biomater,2013,101(4):591-598.
[14]Briem D,Strametz S,Schr9der K,et al.Response of primary fibroblasts and osteoblasts to plasma treated polyetheretherketone(PEEK)surfaces[J].J Mater Sci Mater Med,2005,16(7):671-677.
[15]Noiset O,Schneider YJ,Marchand-Brynaert J.Fibronectin adsorption or/and covalent grafting on chemically modified PEEK film surfaces[J].J Biomater Sci Polym Ed,1999,10(6):657-677.
[16]Noiset O,Schneider YJ,Marchand-Brynaert J.Adhesion and growth of Ca Co2cells on surface-modified PEEK substrata[J].J Biomater Sci Polym Ed,2000,11(7):767-786.
[17]Jger M,Zilkens C,Zanger K,et al.Significance of nanoand microtopography for cell-surface interactions in orthopaedic implants[J].J Biomed Biotechnol,2007,2007(8):69036.
[18]Zhang JY,Dong LL,XU WC,et al.Effect of SO2controlled release packaging on preservation performance of cherry[J].Pack Eng,2013,34(15):45-49.
[19]Meng Z,Liu Y,Wu D.Effect of sulfur dioxide inhalation on cytokine levels in lungs and serum of mice[J].Inhal Toxicol,2005,17(6):303-307.