Ge Yongcheng, Zhao Ting, Fan Sizheng, Liu Pengyuan, Liu Xiaoqiu
Department of Geriatric Stomatology, Hospital of Stomatology, Jilin University, Changchun, 130021, China.
Jilin Provincial Key Laboratory of Tooth Development and Bone Remodeling, Hospital of Stomatology, Jilin University, Changchun, 130021, China.
BMC Oral Health. 2025 Jun 7;25(1):940. doi: 10.1186/s12903-025-06305-7.
This study evaluated the effects of three surface treatments-concentrated HSO, sodium borohydride (NaBH), and their combination-on the shear bond strengths between polyether ether ketone (PEEK) and both composite resins and poly(methyl methacrylate) (PMMA).
PEEK specimens (n = 160) were randomly assigned to composite resin and PMMA groups, each of which was subdivided into normal and aging groups (n = 40), each comprising samples that were pristine (untreated) or treated with dimethyl sulfoxide (DMSO), NaBH, or concentrated HSO or sequentially treated with NaBH and concentrated HSO (n = 8). The shear bond strength (SBS) of the normal and aged specimens were measured. For the normal and treated specimens, the surface and cross-sectional morphologies were analyzed using scanning electron microscopy (SEM), the chemical bond modifications were investigated using X-ray photoelectron and attenuated total reflectance Fourier-transform infrared spectroscopies (XPS and ATR-FTIR, respectively), the mechanical strengths were measured using three-point bending tests, and the cytotoxicities were evaluated using cell-counting kit-8 (CCK-8) assays and 4',6-diamidino-2-phenylindole (DAPI) staining.
NaBH etched the PEEK surface, generating a fibrous texture, while concentrated HSO produced a surface possessing variously sized pores. Sequential treatment with NaBH and concentrated HSO produced dense, permeating pores. XPS confirmed that NaBH reduced carbonyl groups to hydroxyl groups on the PEEK surface. ATR-FTIR spectroscopy confirmed that the silane coupling agent grafted onto the PEEK surface, forming Si-O-C bonds. NaBH and concentrated HSO both strengthened the shear bonding between the PEEK and both the composite resins and PMMA (P < 0.05). The specimens sequentially treated with NaBH and 98% concentrated HSO possessed the strongest shear bonding (P < 0.05). The aged specimens sequentially treated with NaBH and concentrated HSO retained very strong shear bonds. CCK-8 cytotoxicity assays and DAPI staining confirmed that these surface treatments meet oral biocompatibility standards.
NaBH introduced chemical bonds to the PEEK surface, while concentrated-HSO-induced sulfonation enhanced the micromechanical interlocking between the PEEK and both the composite resins and PMMA. These combined physicochemical modifications significantly strengthened the adhesion between the PEEK and both the composite resins and PMMA and effectively strengthened PEEK's bonding.
本研究评估了三种表面处理方法——浓硫酸(HSO)、硼氢化钠(NaBH)及其组合——对聚醚醚酮(PEEK)与复合树脂和聚甲基丙烯酸甲酯(PMMA)之间剪切粘结强度的影响。
将160个PEEK样本随机分为复合树脂组和PMMA组,每组再分为正常组和老化组(每组n = 40),每组包括原始(未处理)样本或用二甲基亚砜(DMSO)、NaBH、浓硫酸处理的样本,或依次用NaBH和浓硫酸处理的样本(n = 8)。测量正常和老化样本的剪切粘结强度(SBS)。对于正常和处理后的样本,使用扫描电子显微镜(SEM)分析表面和横截面形态,分别使用X射线光电子能谱和衰减全反射傅里叶变换红外光谱(分别为XPS和ATR - FTIR)研究化学键修饰,使用三点弯曲试验测量机械强度,并使用细胞计数试剂盒 - 8(CCK - 8)测定法和4',6 - 二脒基 - 2 - 苯基吲哚(DAPI)染色评估细胞毒性。
NaBH蚀刻PEEK表面,产生纤维状纹理,而浓硫酸产生具有各种尺寸孔隙的表面。依次用NaBH和浓硫酸处理产生致密、渗透的孔隙。XPS证实NaBH将PEEK表面的羰基还原为羟基。ATR - FTIR光谱证实硅烷偶联剂接枝到PEEK表面,形成Si - O - C键。NaBH和浓硫酸均增强了PEEK与复合树脂和PMMA之间的剪切粘结(P < 0.05)。依次用NaBH和98%浓硫酸处理的样本具有最强的剪切粘结力(P < 0.05)。依次用NaBH和浓硫酸处理的老化样本保留了非常强的剪切粘结力。CCK - 8细胞毒性测定法和DAPI染色证实这些表面处理符合口腔生物相容性标准。
NaBH在PEEK表面引入化学键,而浓硫酸诱导的磺化增强了PEEK与复合树脂和PMMA之间的微机械互锁。这些组合的物理化学修饰显著增强了PEEK与复合树脂和PMMA之间的粘附力,并有效地增强了PEEK的粘结力。