Calcium silicate hydrate（C-S-H） with Ca/Si ratio 1.0 was prepared via precipitation in solution and heated at various temperatures to investigate its dehydration behavior. The dehydration, structural collapse and recrystallization characteristics of C-S-H and its microstructural change during heating process were investigated by XRD, SEM, Raman and TG-DSC techniques. C-S-H gradually lost non-evaporable water upon heating, about 50% and 80% non-evaporable water was removed below 200 and 400 ℃, respectively, and the rest was removed up to about 1 000 ℃. At 400 ℃, dehydrated C-S-H exhibited the increasing disordering of calcium/silicon environment and the decreasing symmetrical bending vibration of Si-O-Si of Q^2 silicate chains. At 650 ℃ non-bridging oxygen atoms（O（non）） attached to silicon were almost removed, and significant structural change occurred, and at 815 ℃ C-S-H dehydrated to wollastonite.
The effects of polyaerylamide （PAM） and polyvinyl alcohol （PVA） on morphology and structure of calcium silica~ hydrate with C/S 1.0-1.7 prepared via precipitation in solution were investigated by XRD, FT-IR and TEM techniques. The results show that incorporation of the polymers decreased the order degree, increased the interlayer spacing and disturbed the layered stacking of C-S-H. Interlayer spacing expansion depended on C/S ratios and type of polymer. Interlayer spacing expansion had a minimum at C/S 1.0 and a maximum at C/S 1.3 and 1.5. Interlayer spacing expansion of PAM was bigger than that of PVA with the same C/S. C-S-H added with PVA mainly exhibited foil-like and fibrillar morphology. The fibrils were of variable length from a few tens of nanometers to a few hundreds of nanometers. Fibrils or foils seemed to be longer in the presence of PVA.
制备了具有宽范围Ca/(Si+Al)比和Al/Si比的铝掺杂水化硅酸钙(C-A-S-H)系列样品,采用^(27)Al魔角旋转固体核磁共振技术(^(27)Al MAS NMR)半定量研究了Al在C-A-S-H结构中的配位状态。结果表明:Al在C-A-S-H结构的配位形式和位置主要取决于其初始Ca/(Si+Al)比和Al/Si比。当初始Ca/(Si+Al)比低时(0.6和0.8),Al只能取代硅酸盐链硅氧四面体结构中四配位的Si,以Al[4]的形式存在;随着Ca/(Si+Al)比的增加,部分Al开始形成Al[5]和Al[6],且随着Al/Si比的增加,Al[4]的含量减小,Al[5]和Al[6]的总量增加,但Al[4]还是占主要比例,Al[5]的量非常少。Al[4]既可取代桥四面体中的Si也可取代配对四面体中的Si,但优先取代的是桥四面体中的Si,两者取代比并非恒定,而是随着初始Ca/(Si+Al)比和Al/Si比的变化而变化。
Micro computed tomography (Micro-CT) was applied to obtain three-dimensional images of the microstructure of cement paste (water-to-cement mass ratio of 0.5) at different ages. By using the Amira software, component phases of the cement paste such as pores, hydration products, and unhydrated clinker particles were segmented from each other based on their 3D image grey levels; their relative contents were also calculated with the software, and the data are 61.2%, 0% and 38.8% at the beginning of hydration and 11.8%, 78.5% and 9.7% at 28 d age, respectively. The hydration degree of cement paste at different ages was compared with the experimental data acquired by loss on ignition (LOI) tests. The results show that the calculated and measured data reasonably agree with each other, which indicates that micro-CT is a useful and reliable approach to characterize the micro structure evolution of hydrating cement paste.
