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使用魔角核磁共振(MAS-NMR)对商用离聚物玻璃进行表征。

Characterisation of commercial ionomer glasses using magic angle nuclear magnetic resonance (MAS-NMR).

作者信息

Stamboulis Artemis, Law Robert V, Hill Robert G

机构信息

Department of Materials, Imperial College, Prince Consort Road, London SW7 2BP, UK.

出版信息

Biomaterials. 2004 Aug;25(17):3907-13. doi: 10.1016/j.biomaterials.2003.10.074.

Abstract

Five commercial ionomer glasses (Fuji IX, Ketac Molar, G338, G2, and G2SR) used to produce glass (ionomer) polyalkenoate dental cements were studied. 29Si, 27Al, 31P and 19F magic angle spinning nuclear magnetic resonance (MAS-NMR) Spectroscopy was used to characterise the glasses and the resulting spectra compared with previous studies of model glasses. The 29Si NMR spectra were consistent with Q4(3Al) and Q4(4Al) units being present and agreed with the low non-bridging oxygen contents calculated from the elemental composition. The 27Al NMR spectra typically exhibited three distinct sites at 45-60, 20 and 0 ppm which have been attributed to Al(IV), Al(V) and Al(VI) coordinate aluminium. The presence of Al(V) and Al(VI) are consistent with previous studies of model ionomer glasses. The 31P spectra all exhibited a chemical shift between -8 and -23 ppm with the exception of the Ketac Molar glass, which exhibited a peak at 2-3 ppm consistent with orthophosphate. The chemical shift of 31P in the range -8 to -23 ppm indicates a PO(4) tetrahedra surrounded by 1-4 Al moieties. The (19)F NMR spectra indicated the presence of Al-F-Ca(n) in the G2 and G338 glasses, Al-F-Sr(n) in the G2SR and Fuji IX glasses and crystalline CaF2, LaF3, Al-F-Ca(n) in the Ketac Molar glass. The G338 glass with a high non-bridging oxygen content showed the presence of a F-Ca(n) species. There was also present in all the glasses a peak corresponding to Al-F-Na(n). The intensity of this peak was approximately proportional to the sodium content.

摘要

对用于生产玻璃(离聚物)聚羧酸锌水门汀的五种商用离聚物玻璃(富士IX、克塔摩拉、G338、G2和G2SR)进行了研究。采用29Si、27Al、31P和19F魔角旋转核磁共振(MAS-NMR)光谱对玻璃进行表征,并将所得光谱与之前对模型玻璃的研究进行比较。29Si NMR光谱与存在的Q4(3Al)和Q4(4Al)单元一致,并且与根据元素组成计算出的低非桥氧含量相符。27Al NMR光谱通常在45 - 60、20和0 ppm处表现出三个不同的位点,这已归因于Al(IV)、Al(V)和Al(VI)配位铝。Al(V)和Al(VI)的存在与之前对模型离聚物玻璃的研究一致。除克塔摩拉玻璃外,所有31P光谱的化学位移均在 - 8至 - 23 ppm之间,克塔摩拉玻璃在2 - 3 ppm处出现一个与正磷酸盐一致的峰。31P在 - 8至 - 23 ppm范围内的化学位移表明PO(4)四面体被1 - 4个Al部分包围。19F NMR光谱表明G2和G338玻璃中存在Al-F-Ca(n),G2SR和富士IX玻璃中存在Al-F-Sr(n),克塔摩拉玻璃中存在结晶CaF2、LaF3、Al-F-Ca(n)。具有高非桥氧含量的G338玻璃显示出F-Ca(n)物种的存在。所有玻璃中还存在一个与Al-F-Na(n)相对应的峰。该峰的强度大致与钠含量成正比。

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