Table 4.
QCM-D | |||||
---|---|---|---|---|---|
Mass, m [ng cm−2] |
Thickness, d [nm] |
Surface concentration, Γtheor [mol cm−2] (MSiO2 = 60.1 g mol−1) |
Surface concentration, Γtheor [mol cm−2] (MH4SiO4 = 96.1 g mol−1) |
Number zQCM-D of adsorbed Si—O—Si layers |
|
pH 7.2, K2HPO4/KH2PO4 | |||||
EDC | 1355 ± 32 | 6.8 ± 0.9 | 22.5 × 10−9 | 14.1 × 10−9 | 21.5 ± 0.5 |
EDC/EDA | 502 ± 14.2 | 2.5 ± 0.4 | 8.35 × 10−9 | 5.22 × 10−9 | 8.0 ± 0.5 |
Non-activated | 370 ± 10.6 | 1.9 ± 0.3 | 6.16 × 10−9 | 3.85 × 10−9 | 5.5 ± 0.5 |
pH 7.2, KOH | |||||
EDC | 219 ± 5.3 | 1.2 ± 0.2 | 3.64 × 10−9 | 2.28 × 10−9 | 4 |
EDC/EDA | 142 ± 3.5 | 0.6 ± 0.1 | 2.36 × 10−9 | 1.48 × 10−9 | 2 |
Non-activated | 46 ± 1.8 | 0.2 ± 0.1 | 0.77 × 10−9 | 0.48 × 10−9 | 1.0 |
FTIR-ATR |
|||||
Surface concentration, Γtheor [mol cm−2] |
Surface concentration, Γexp [mol cm−2] |
Number zQCM-D of adsorbed Si—O—Si layers |
|||
| |||||
pH 7.2, K2HPO4/KH2PO4 | |||||
Non-activated | 9.04 × 10−9 | 3.69 × 10−9 (⊥) | 4.0 ± 0.5 | ||
3.87 × 10−9 (II) |
As basis for the surface concentration Γ a densely spherical package of SiO4 tetrahedra with a Si—O—Si distance of 0.3058 nm (rsphere = 0.1529 nm) was assumed.
QCM-D: surface concentration Γtheor = m/M, number of adsorbed Si—O—Si layers zQCM-D = d/2rSi—O (rSi—O = 0.1529 nm).
FTIR-ATR: surface concentration Γtheor = 4/(Na·a2) with a2: smallest unit cell (a2 = Π·r2, rSi—O = 0.1529 nm), Na: Avogadro constant, surface concentration Γmeas = A·d/(ε·N·ν·de) with A: integrated absorbance of the Si—O—Si band, d: thickness of the adsorbed layer, ε: molar extinction coefficient, N: middle number of intern active reflections, ν: number of functional groups/molecule, de: penetration depth. The molar extinction coefficient ε was calculated from transmission measurements of a (SiO2)x·yH2O gel with the help of the Lambert–Beersche law A = ε·c·dFringes.c: concentration of methanol, dFringes: cell thickness determined by “Fringes” [32], number of adsorbed Si—O—Si layers zFTIR = Γexp/Γtheor.