不同溶剂对MDP提高氧化锆陶瓷粘接性能的影响

目的评价磷酸酯单体MDP在几种不同的溶剂环境中对提高氧化锆陶瓷与树脂粘接效果的影响。方法配置MDP的乙醇、丙酮和乙醇/丙酮(1∶1)溶液作为实验性底涂剂,对比这几种底涂剂处理氧化锆陶瓷后与树脂的粘接强度,测试以不应用任何底涂剂作为阴性对照组,以应用市场常用包含MDP的底涂剂产品作为阳性对照组。使用X线光电子能谱分析检测实验性底涂剂处理氧化锆陶瓷后表面新形成的化学键。结果未应用底涂剂组显示了最低的粘接强度值,当前实验中的3种溶剂的底涂剂显示了较高的粘接强度值,但各组间并无统计学差别。X线光电子能谱分析在几种实验性底涂剂处理的氧化锆表面均检测出"-P-O-Zr"键。结论以丙酮、乙醇或两者混合液作为溶剂时MDP均能提高氧化锆陶瓷与树脂的粘接强度。     

热酸溶液蚀刻对氧化锆粘接强度的影响

目的 研究牙科氧化锆经3种酸溶液加热处理后与树脂的初期粘接强度和粘接耐久性。方法 将80枚氧化锆瓷片分为5组,进行不同的表面处理,随后制作陶瓷/树脂粘接试样。其中,A组：经H2SO4/（NH4）2SO4混合液热处理,使用氧化锆底涂剂;B组：HF/HNO3混合液热处理,使用氧化锆底涂剂;C组：经H2SO4/HF/HNO3混合液热处理,使用氧化锆底涂剂;D组：氧化铝喷砂,使用氧化锆底涂剂;E组：摩擦化学法硅涂层,使用硅烷偶联剂。将粘接试样分为两部分,分别于水储24 h和40 d后进行剪切粘接强度（SBS）测试。扫描电镜（SEM）下观察3种酸处理和氧化铝喷砂处理氧化锆瓷片的表面形态。结果 老化前E组SBS最高,其余4组间差异无统计学意义;老化后A、B、E组显示了较高的SBS。水储老化40 d后A组和B组的SBS值较水储24 h时有显著性增加,剩余3组老化前后差异均无统计学意义。结论 热酸溶液蚀刻相对于喷砂的粗化方法能够显著提高氧化锆与树脂的初期粘接强度和粘接耐久性。     

磷酸酯类单体与氧化锆间化学反应模型的建立及作用机制

目的 对磷酸酯单体10-甲基丙烯酰氧癸二氢磷酸酯（MDP）提高四方相氧化锆与树脂间化学粘接的作用机制进行解释。方法 分别构建MDP、四方相氧化锆陶瓷晶体以及两者反应的数字模型,采用热力学方法对MDP分子与四方相氧化锆晶体簇相互作用的吉布斯自由能和平衡常数进行计算。结果MDP与四方相氧化锆晶体簇可能发生单配位形式和双配位形式的结合,其吉布斯自由能分别为-147.761和-158.073 kJ·mol^-1,说明MDP能够与四方相氧化锆晶体发生化学结合,平衡常数较高（4.95×10²⁷）的双配位结合形式较平衡常数较低（7.72×10²⁵）的单配位结合形式更为稳定。结论 MDP能够通过与四方相氧化锆陶瓷以双配位形式发生化学结合来提高其与树脂的粘接强度。     

磷酸酯单体对口腔氧化锆陶瓷粘接耐久性的影响

目的探讨含甲基丙烯酰癸基二氢磷酸酯(methacryloyloxydecyl dihydrogen phosphate,MDP)的底涂剂、通用粘接剂和自粘接树脂水门汀对口腔氧化锆陶瓷粘接耐久性的影响。方法制作氧化钇稳定的四方相氧化锆瓷片210个,氧化铝表面喷砂后分为7组(每组30个),以不含MDP的传统树脂水门汀作为对照组,其余6组分别应用两种含MDP的氧化锆底涂剂联合传统树脂水门汀(底涂剂组)、两种含MDP的通用粘接剂联合传统树脂水门汀以(粘接剂组)及两种含MDP的自粘接树脂水门汀(自粘接树脂水门订组),粘接氧化锆瓷片和复合树脂,制作粘接试件。试件制成后每组半数37℃水储存24 h(老化前),另一半37℃水储存12个月(老化后);测试剪切强度(即粘接强度)并分析断裂模式。结果水储存老化前与对照组较低的粘接强度[(5.04±0.50)MPa]相比,其他6组粘接强度均显著增加(P<0.05),均可达到9.51 MPa以上;其中2个自粘接树脂水门汀组粘接强度均较高,最大为(11.06±0.84)MPa。水储存老化后各组粘接强度均比老化前显著降低(P<0.05),除对照组外,其余6组粘接强度仍在7.44 MPa以上;其中2个自粘接树脂水门汀组及1个粘接剂组维持较高的粘接效果,且与2个底涂剂组的差异均有统计学意义(P<0.05)。结论含MDP的产品可提高口腔氧化锆陶瓷的粘接耐久性,且不同产品类型对口腔氧化锆陶瓷粘接耐久性有不同的影响。     

不同类型钛酸酯偶联剂对氧化锆陶瓷与树脂初期粘接强度的影响

目的评价几种不同类型的钛酸酯偶联剂(KR-TTS、KR-12、KR-38S)单独使用或结合两种不同磷酸酯单体(MDP、PENTA)对牙科氧化锆陶瓷与树脂粘接强度的影响。方法将130枚氧化锆瓷片喷砂处理后随机分为13组,各组分别使用以下方法进行表面处理:单纯包含一种钛酸酯偶联剂的自配底涂剂(KR-TTS,组Kt)、(KR-12,组K1)、(KR-38S,组K_3)处理;包含钛酸酯偶联剂分别与磷酸酯单体MDP或PENTA组合的自配底涂剂(组MKT-PK_3)处理;包含磷酸酯单体MDP(组M)或PENTA(组P)的自配底涂剂,以及商品化含MDP的底涂剂产品Z-Prime Plus(组Z)处理作为阳性对照组;喷砂处理后不使用底涂剂作为阴性对照组(组C0)。以上表面处理后的瓷片制作粘接试件,37℃水储24 h后测试剪切粘接强度。结果各类型的钛酸酯偶联剂无论是单独使用,还是与磷酸酯单体(MDP,PENTA)组合使用,获得的剪切粘接强度均低于单独以磷酸酯单体MDP或PENTA自配的底涂剂或Z-Prime Plus处理组(P<0.05),部分使用钛酸酯偶联剂组的剪切粘接强度甚至低于单纯喷砂组。结论钛酸酯偶联剂会负面影响氧化锆陶瓷与树脂的粘接性能。     

MDP对氧化锆陶瓷粘接性能的提高及微渗漏评价

目的评价两种包含磷酸酯单体MDP的氧化锆底涂剂结合或不结合喷砂处理对提高氧化锆陶瓷与树脂粘接强度和边缘封闭的影响。方法对比氧化锆陶瓷应用包含MDP的氧化锆底涂剂结合或不结合氧化铝喷砂处理时对树脂的粘接强度。单纯对氧化锆陶瓷进行氧化铝喷砂处理作为阴性对照组。使用亚甲基蓝染色法评价以上不同处理的氧化锆与树脂间的微渗漏情况。结果单纯喷砂处理显示了最低的粘接强度,应用包含MDP的氧化锆底涂剂能够增加氧化锆陶瓷与树脂的粘接强度,在应用底涂剂前进行氧化铝喷砂处理能够进一步增加与树脂的粘接强度。单纯喷砂组显示了最严重的微渗漏,应用包含MDP的底涂剂时,不论是否经过喷砂处理,微渗漏程度均降低。结论喷砂结合氧化锆底涂剂是提高氧化锆陶瓷粘接的较好方法。     

不同表面处理方法对氧化锆陶瓷微观结构和粘接强度影响的研究

目的 研究不同机械-化学性表面处理对氧化锆陶瓷表面微观形貌、结构及组成的影响,比较不同表面改性后的氧化锆陶瓷与人牙本质的粘接强度。方法 选择氧化锆陶瓷（IPS e.max ZirCAD）,切割并烧结形成长6 mm、宽6 mm、高5 mm瓷块126块,随机分为7组,每组18块,分别进行如下处理。A组：不处理,对照组;B组：50 μm氧化铝喷砂;C组：50 μm氧化铝喷砂+30 μm二氧化硅蚀刻;D组：50 μm氧化铝喷砂+30%硅溶胶涂层;E组：110 μm氧化铝喷砂;F组：110 μm氧化铝喷砂+30 μm二氧化硅蚀刻;G组：110 μm氧化铝喷砂+30%硅溶胶涂层。每组随机抽取2个试件,分别用表面粗糙度轮廓仪测量表面粗糙度（R_a）,X射线衍射（XRD）观察表面晶相结构,能谱分析仪（EDX）分析表面化学元素组成,扫描电镜（SEM）观察表面微观形貌。收集70颗人离体第三磨牙制备成牙本质平面。使用双固化树脂水门汀将氧化锆试件与牙本质平面粘接,万能试验机进行剪切粘接强度（SBS）测试。采用SPSS 17.0软件对结果进行单因素方差分析及多重检验。结果 与对照组相比,表面处理后的氧化锆陶瓷R_a具有显著性差异（P<0.05）。所有表面处理后都发生了四方相（t）到单斜相（m）的晶相转换,且热处理后的m相体积分数最多。表面改性后化学元素组成发生变化,EDX结果显示硅涂层后,硅元素含量显著升高,Zr、Y、Hf减少。SEM图像显示,氧化铝喷砂后的氧化锆陶瓷表面出现一些微小断裂、晶界消失;硅溶胶薄膜烧结后体积明显收缩,可见裂纹与剥离。不同表面处理组的粘接强度有统计学差异（P<0.05）,F和G组SBS值最大,其次为C和D组,显著大于B和E组（P<0.05）,对照组的SBS值最小（P<0.05）。结论 氧化铝喷砂、硅粉蚀刻、硅溶胶涂层法可显著改变氧化锆陶瓷的表面形貌、结构和组成,有利于氧化锆陶瓷与牙体组织粘接时形成微机械嵌合与化学结合作用。氧化铝喷砂后硅涂层处理是一种比较理想的表面改性方法,可显著提高氧化锆陶瓷与牙体组织的粘接强度。     

一种自粘接树脂水门汀与氧化锆陶瓷粘接的耐久性评价

目的评价一种自粘接树脂水门汀RelyX~(TM) U_(200)与氧化锆陶瓷粘接的强度和耐久性。方法 90枚氧化锆瓷片(Y-TZP)喷砂处理后分别以"使用自粘接树脂水门汀RelyX~(TM) U_(200)(RU组)"和"氧化锆底涂剂处理+使用传统树脂水门汀RelyX Veneer(ZPRV组,对照组)"两种粘接策略制作Y-TZP/树脂水门汀/光固化复合树脂结构的粘接试件。两组试件分别按照以下三种方法进行处理:37℃水储24 h,30 000次冷热循环下进行人工老化,37℃水储6个月进行人工老化,随后测试试件的剪切粘接强度,分析断裂模式。按照剪切测试同样的两种粘接策略分别制作双瓷层粘接试件(n=10),以去离子水浸泡,电感耦合等离子体质谱(ICP-MS)测试1、7、14、21、30、60和90 d的磷元素释放量。结果两种粘接策略提供了类似的氧化锆陶瓷与树脂间的粘接强度(P=0.841),这一粘接强度在老化处理后均降低(P<0.05),并且老化处理后各组试件的粘接断裂模式所占比例增加。RU组可获得与ZPRV组相等或更高的粘接耐久性。ICP-MS测试仅在Ctr-RU(单纯树脂水门汀RelyX~(TM) U_(200),对照组)、RU和ZPRV中检测到了磷元素的释放,随浸泡时间的延长,磷元素的释放呈现一定的增加。结论 RelyX~(TM) U_(200)树脂水门汀在无需底涂剂处理的条件下用于氧化锆陶瓷粘接可获得较好的粘接强度和粘接耐久性。     

通用型粘接剂和树脂水门汀对氧化锆 剪切粘接强度的影响

目的 研究通用型粘接剂和树脂水门汀对氧化锆陶瓷剪切粘接强度和耐久性的影响。方法 氧化锆陶瓷烧结制作20 mm×10 mm×10 mm和10 mm×10 mm×10mm两种尺寸的试件,实验分为12组,将这2种试件分别采用不同的树脂水门汀（RelyX Ultimate树脂水门汀、Clearfil SAC自粘接树脂水门汀）和通用粘接剂（无粘接剂、Scotchbond通用粘接剂、Clearfil SE One粘接剂）在不同的储存条件（水浴、水浴+冷热循环）下进行粘接。测试剪切粘接强度,分析断裂形态。结果 水门汀（F=8.41,P<0.01）和粘接剂（F=30.34,P<0.01）对氧化锆剪切粘接强度的影响有统计学意义;储存条件对剪切粘接强度的影响无统计学意义（F=1.83,P=0.18）。RelyX Ultimate树脂水门汀、无粘接剂、水浴+冷热循环储存时的剪切粘接强度最低（14.02 MPa±6.86 MPa）,RelyX Ultimate树脂水门汀、Scotchbond通用粘接剂、水浴+冷热循环储存时的剪切粘接强度最高（54.12 MPa±8.37 MPa）。结论 通用型粘接剂可提高树脂水门汀对氧化锆的粘接耐久性。非自粘接的树脂水门汀如不使用通用型粘接剂则其粘接耐久性下降。     

通用型粘接剂和树脂水门汀对氧化锆剪切粘接强度的影响

目的 研究通用型粘接剂和树脂水门汀对氧化锆陶瓷剪切粘接强度和耐久性的影响。方法 氧化锆陶瓷烧结制作20 mm×10 mm×10 mm和10 mm×10 mm×10mm两种尺寸的试件,实验分为12组,将这2种试件分别采用不同的树脂水门汀（RelyX Ultimate树脂水门汀、Clearfil SAC自粘接树脂水门汀）和通用粘接剂（无粘接剂、Scotchbond通用粘接剂、Clearfil SE One粘接剂）在不同的储存条件（水浴、水浴+冷热循环）下进行粘接。测试剪切粘接强度,分析断裂形态。结果 水门汀（F=8.41,P<0.01）和粘接剂（F=30.34,P<0.01）对氧化锆剪切粘接强度的影响有统计学意义;储存条件对剪切粘接强度的影响无统计学意义（F=1.83,P=0.18）。RelyX Ultimate树脂水门汀、无粘接剂、水浴+冷热循环储存时的剪切粘接强度最低（14.02 MPa±6.86 MPa）,RelyX Ultimate树脂水门汀、Scotchbond通用粘接剂、水浴+冷热循环储存时的剪切粘接强度最高（54.12 MPa±8.37 MPa）。结论 通用型粘接剂可提高树脂水门汀对氧化锆的粘接耐久性。非自粘接的树脂水门汀如不使用通用型粘接剂则其粘接耐久性下降。     

碱性环境下放置的磷酸酯单体对氧化锆陶瓷粘接的作用

目的 研究两种不同的磷酸酯单体MDP、PENTA在碱性环境下放置不同时间对氧化锆陶瓷与树脂间粘接效果的影响。 方法 分别配置含有MDP和PENTA两种磷酸酯单体的处理剂,与一定量的氢氧化钠碱液混合调节pH值为9,以不混合碱液者作为对照,以上处理剂放置2 h、1周、4周后用于处理氧化锆陶瓷,测量与树脂的剪切粘接强度（SBS）。放置不同时间的处理剂处理的氧化锆陶瓷粉以红外光谱分析表面化学键变化（FTIR）。 结果 不论何种磷酸酯单体,混合碱液后均导致氧化锆与树脂间的SBS值降低;不同磷酸酯单体的处理剂增强氧化锆陶瓷与树脂粘接的效果之间不存在统计学差别。 结论 磷酸酯单体混合碱液后对氧化锆与树脂间的粘接强度有负面影响。     

摩擦化学法硅涂层对氧化锆陶瓷粘接强度的影响

目的： 评估摩擦化学法硅涂层对氧化锆陶瓷粘接强度的影响。方法： 将切割烧结后的Lava氧化锆瓷块60件分为6组，每2组分别经喷砂/硅烷偶联剂、喷砂/CoJet Sand/硅烷偶联剂、无处理3种表面处理后，相同表面处理的2组中，每组分别用RelyX Unicem或Panavia F2.0与牙釉质粘接。各组随机抽取5件共30件进行24 h水浴，其余30件进行5000周水热循环，然后进行剪切粘接强度测试。采用SPSS 23.0软件包对数据进行双因素方差分析、Tukey HSD多重比较法及t检验。结果： 喷砂/CoJet/硅烷组的剪切强度均显著高于其他2组（P<0.001）；经老化试验后，喷砂/CoJet/硅烷组使用RelyX Unicem仍保持较高的剪切强度[(21.374±4.433)MPa]，与其他各组相比有显著差异（P<0.001）。结论： 摩擦化学法硅涂层能够有效提高氧化锆的粘接强度及耐久性，表面处理方式与粘接剂之间的相互作用需得到临床关注。     

Effect of silane and MDP-based primers on physico-chemical properties of zirconia and its bond strength to resin cement

ObjectiveTo evaluate the effect of surface treatments on yttria-tetragonal zirconia polycrystal (Y-TZP) characteristics and on resin-mediated zirconia bond.MethodsY-TZP slabs were grit blasted with 45 μm alumina or with 30 μm silica-coated alumina particles. The chemical treatments were: no-chemical treatment (NC), silane-containing primer (SP), MDP (10-Methacryloyloxydecyl dihydrogen phosphate) and silane-containing primer (MPS), MDP-containing primer (MP) and MDP and silane-containing adhesive (MPA). Contact angle as a function of surface roughness (θ_m) and surface roughness parameter (Sdr) were measured using Fringe Projection Phase Shifting (FPPS). Surface free energy (γ_s^TOT) was calculated with a goniometer. Chemical interaction between primers/adhesive and zirconia was analyzed using time-of-flight secondary ion mass spectrometry (ToF-SIMS). Resin cement microshear bond strength (μSBS) was analyzed at either 24-h or 8-months water storage (37 °C). θ_m values, Sdr values, γ_s^TOT and μSBS values were analyzed using Analysis of variance (ANOVA) and post hoc Tukey test (α = 0.05).ResultsChemical treatment had an effect (p < 0.001) on all surface parameters analyzed: θ_m, γ_s^TOT and Sdr. MP-treated group showed higher incidence of P–O–Zr bonds than the other groups, indicating more chemical linkages. Grit blasting (p < 0.001) and the interaction chemical treatment*storage (p < 0.001) did not affect μSBS; all silane-containing primers showed significant drop in μSBS after aging.SignificanceMDP and/or silane-based solutions affect the physicochemical properties of blasted-zirconia. An MDP-based primer is fundamental to achieve a stable resin-zirconia bonding, but the chemical reactivity of MDP is impaired when this molecule is present in a multicomponent system.     

Influence of different surface treatments on the short-term bond strength and durability between a zirconia post and a composite resin core material

STATEMENT OF PROBLEM: Reliable bonding between zirconia posts and composite resin core materials is difficult to achieve because of the smooth surface texture and lack of silica content of zirconia posts. PURPOSE: The purpose of this study was to evaluate the effect of different surface treatments on the short-term bond strength and durability between a zirconia post and a composite resin core material. MATERIAL AND METHODS: Eighty zirconia posts were divided into 4 groups (n=20). Specimens received 1 of 4 different surface treatments: group AIRB, airborne-particle abrasion; group TSC-SIL, tribochemical silica coating (CoJet system) and silanization (ESPE Sil); group AIRB-BSIL, airborne-particle abrasion and MDP-containing primer (Clearfil SE Bond Primer)/silane coupling agent (Clearfil Porcelain Bond Activator) mixture application; and group TSC-BSIL, tribochemical silica coating and MDP-containing primer/silane coupling agent mixture application. Average surface roughness (Ra) of zirconia posts produced by airborne-particle abrasion or silica coating was measured using an optical profilometer. Composite resin core foundations (Build-it FR) were formed using transparent acrylic resin tubes (12mm in length and 7mm in diameter). Each group was further divided into 2 subgroups of 10 specimens and stored in distilled water at 37 degrees C, either for 24 hours or for 150 days with 37,500 thermal cycles between 5 degrees C and 55 degrees C, with a dwell time of 30 seconds. Following water storage, the specimens were sectioned perpendicular to the bonded interface into 2-mm-thick post-and-core specimens under water cooling. Push-out tests were performed with a universal testing machine at a crosshead speed of 0.5mm/min. Debonded post surfaces were examined with SEM. Data were analyzed with 1- and 2-way ANOVA and Tukey multiple comparison tests (alpha=0.05). RESULTS: No significant differences were detected between the Ra values of airborne-particle-abraded and silica-coated specimens (P=.781). The short-term mean bond strengths for group TSC-BSIL (27.1 +/- 3.2 MPa) and TSC-SIL (25.2 +/- 2.4 MPa) were statistically higher (P<.001) than AIRB-BSIL (23.3 +/- 2.2 MPa). The relatively high bond strengths for groups TSC-BSIL and TSC-SIL decreased significantly after 150 days of water storage to 13.5 +/- 1.6 and 11.8 +/- 1.2 MPa, respectively (P<.001). Durable bonding was obtained only in group AIRB-BSIL (21.8 +/- 2.7 MPa), which was also the only group demonstrating predominantly cohesive failures in the core material after long-term water storage. CONCLUSIONS: Data suggest that the short-term high bond strength obtained with a silane coupling agent or MPD-containing primer/silane coupling agent mixture to silica-coated zirconia posts was decreased with water storage and thermal cycling, whereas a durable bond could be obtained when an MPD-containing primer/silane coupling agent mixture was applied to the airborne-particle-abraded post surface.     

氧化锆处理剂和自粘接树脂水门汀对氧化锆陶瓷粘接的效果评价

目的 评价包含酸性功能单体的氧化锆处理剂和自粘接树脂水门汀对氧化锆陶瓷粘接强度提高的效果。方法 制作80枚氧化锆瓷片,粘接面以氧化铝喷砂后分为5组,分别为C组、R组、S组、ZC组、ZR组,其中S组应用溶胶凝胶法制备硅涂层后以硅烷偶联剂处理,ZC组和ZR组以氧化锆处理剂Z-Prime Plus处理。再制作80枚复合树脂圆片,将其粘接于处理后的陶瓷表面,C组、S组、ZC组使用传统双酚A双甲基丙烯酸缩水甘油酯（Bis-GMA）树脂水门汀,R组、ZR组使用自粘接树脂水门汀。各组粘接试件又分为两亚组,分别于冷热循环前后测试剪切粘接强度（SBS）。以红外光谱和气相质谱分析表征氧化锆处理剂。结果 C组的SBS值最低,R组、ZC组和ZR组较高。冷热循环对SBS无显著影响。红外光谱分析可见,Z-Prime Plus中包含苯环、羰基等结构。气相质谱分析可知,Z-Prime Plus中包含2-甲基丙烯酸羟乙酯、三乙胺等成分。结论 氧化锆处理剂和自粘接树脂水门汀的使用提高了氧化锆陶瓷的粘接性能。     

Interaction of silane with 10-MDP on affecting surface chemistry and resin bonding of zirconia

ObjectiveTo investigate the effect of silane contents on their chemical interaction with 10-methacryloyloxydecyl-dihydrogen phosphate (MDP), and affecting the bonding of MDP to zirconia by time-of-flight secondary ion mass spectrometry (TOF-SIMS) and solid-state nuclear magnetic resonance (SSNMR) spectroscopy.MethodsZirconia (Cercon ht, Dentsply) slabs were prepared and fully sintered. Experimental primers SE-5 and SE-10 were formulated by adding 5 wt% and 10 wt% γ-methacryloxypropyltrimethoxysilane to an MDP-based primer SE BOND (SE), respectively. SE, SE-5, and SE-10 were applied on the assigned zirconia slabs. The chemical compositions on the surface and adhesive interfaces were examined by TOF-SIMS in a depth-profiling mode. Hydrophilicity and resin affinity of treated zirconia were analyzed. The bond strengths to resin cylinder were examined either after 24-h storage or thermocycles. In addition, zirconia powders treated with three primers were assessed by SSNMR spectrometry for the adsorption of MDP.ResultsTOF-SIMS analysis showed that SE treatment generated the greatest amount of P-O-Zr related ions, which reduced in SE-5 and SE-10 groups. The 3D ion-images illustrated the generation of ZrO₂(OH)^- ions with silane contents. The SSNMR analysis revealed that the chemical bonding was mainly P-O-Zr ionic bonds in SE but shifted to P-OH-Zr hydrogen bonds in SE-5 and SE-10. SE-5 and SE-10 treated zirconia presented higher hydrophilicity and affinity to resin compared to Zr did. SE showed the highest initial bond strength which significantly decreased after thermocycling.SignificanceMDP adsorption onto zirconia via P-O-Zr ionic bond promotes bonding with resin. The silane enhances the hydroxylation of zirconia and impairs the adsorption of MDP, but does not adversely affect the bond durability.     

Effect of cleaning protocol on silica deposition and silica-mediated bonding to Y-TZP

ObjectivesTo evaluate the effect of cleaning methods on the deposition of silica on yttria-stabilized zirconium dioxide (Y-TZP) surface and on the silane-silica mediated bond strength between Y-TZP and resin cement.MethodsY-TZP slabs were air-abraded with 30 μm silica-coated alumina particles and distributed in three groups: no cleaning, cleaning with a stream of oil-free air/water spray for 5 s and cleaning with an ultrasonic bath in water for 10 min. The distribution of Si on the Y-TZP surfaces was recorded using energy dispersive spectroscopy (EDS). After the treatment was applied, Y-TZP slabs (n = 20) received a primer application and resin cement cylinders were built on the surface. After storage (24 h) in water storage or 3 months plus thermocycling; n = 10), microshear bond strength test (μSBS) was performed. X- ray Photoelectron Spectroscopy (XPS) characterized the chemical bonds between the silica layer and the silane-containing primer. Data were analyzed using ANOVA and Tukey test, as well as Weibull analysis (α = 0.05).ResultsCleaning method had a significant effect on the amount of Si deposited on zirconia surface (p < 0.001) and, consequently, on bond strength (p < 0.001). Storage/aging also had a significant effect on bond strength (p < 0.001). Low values of Weibull moduli for bond strength were observed for all groups after aging. XPS showed silane-silica chemical interaction for all groups.SignificanceThe silica deposited by tribochemical coating to Y-TZP was removed by the cleaning methods evaluated, compromising bond strength. Stability of the bonding is also a concern when no cleaning method is applied.     

Comparison of shear test methods for evaluating the bond strength of resin cement to zirconia ceramic

Objective. This study compared the sensitivity of three shear test methods for measuring the shear bond strength (SBS) of resin cement to zirconia ceramic and evaluated the effects of surface treatment methods on the bonding. Materials and methods. Polished zirconia ceramic (Cercon® base, DeguDent) discs were randomly divided into four surface treatment groups: no treatment (C), airborne-particle abrasion (A), conditioning with Alloy primer (Kuraray Medical Co.) (P) and conditioning with Alloy primer after airborne-particle abrasion (AP). The bond strengths of the resin cement (Multilink N, Ivoclar Vivadent) to the zirconia specimens of each surface treatment group were determined by three SBS test methods: the conventional SBS test with direct filling of the mold (Ø 4 mm × 3 mm) with resin cement (Method 1), the conventional SBS test with cementation of composite cylinders (Ø 4 mm × 3 mm) using resin cement (Method 2) and the microshear bond strength (μSBS) test with cementation of composite cylinders (Ø 0.8 mm × 1 mm) using resin cement (Method 3). Results. Both the test method and the surface treatment significantly influenced the SBS values. In Method 3, as the SBS values increased, the coefficients of variation decreased and the Weibull parameters increased. The AP groups showed the highest SBS in all of the test methods. Only in Method 3 did the P group show a higher SBS than the A group. Conclusions. The μSBS test was more sensitive to differentiating the effects of surface treatment methods than the conventional SBS tests. Primer conditioning was a stronger contributing factor for the resin bond to zirconia ceramic than was airborne-particle abrasion.     

表面融附玻璃陶瓷对氧化锆与树脂粘接强度的影响

目的 评估氧化锆玻璃陶瓷表面融附处理后粘接力的变化.方法 将60个氧化锆陶瓷试件平均分为3组,分别接受以下表面处理:50 μm氧化铝喷砂(Sb组);融附玻璃陶瓷(Fu组);氧化铝喷砂后融附玻璃陶瓷(Sb-Fu组).另以20个铸瓷试件作为铸瓷对照组.所有试件应用树脂粘接材料Super bond C＆B粘接在核树脂圆柱上,其中1/2试件经过冷热循环老化(10 000次,5～55℃),测量所有试件的粘接强度.结果 未经过冷热循环处理的Sb、Fu、Sb-Fu和铸瓷对照组试件的粘接强度标准差±均值分别是24.76±2.80、29.08±5.80、28.67±7.20和31.30±2.90 MPa,Sb组的粘接强度明显低于其他3组(P＜0.05),而Fu和Sb-Fu组与铸瓷对照组相比差异无统计学意义;冷热循环后,4组的粘接强度分别是24.45±3.90、28.50±3.70、25.41±2.00和32.19±3.90 MPa,Sb和Sb-Fu组明显低于铸瓷对照组(P＜0.01).Fu和Sb-Fu组多为树脂内聚断裂和混合断裂.结论 玻璃陶瓷融附处理比单纯喷砂更能提高氧化锆的粘接强度.