Multimode 5 afm

The crystal phase was analyzed by powder X-ray diffraction (XRD; Bruker Co., Bremen, Germany) on a D8 Advance diffractometer using Cu Kα radiation (λ = 0.154 Å). The morphology, structure and size of the samples were determined by field-emission scanning electron microscopy (FESEM; Philips XL30 ESEM FEG, Japan) and transmission electron microscopy (TEM; FEI Tecnai G2 S-Twin, München, Germany). The elemental compositions were analyzed by energy-dispersive X-ray energy spectrometry (EDX; Philips, XL-30 W/TMP, Konan, Japan). Fourier transform infrared spectrometry (FT-IR, Bio-Rad Win-IR Spectrometer, Watford, UK) was recorded in the range of 400–4000 cm⁻¹ using the attenuated total reflection (ATR) mode and the KBr slice method. Atom force microscopy (AFM) images were acquired by Bruker’s Dimension Icon and Multimode-V AFM. The amounts of GdPO₄·H₂O, GdPO₄·H₂O@SiO₂, GdPO₄·H₂O@SiO₂–APS, and PBLG-g-GdPO₄·H₂O were determined by thermogravimetric analysis (TGA, TA Instruments TGA500, New Castle, DE, USA) in air at a heating rate of 10 °C/min from 25 °C to 800 °C.

GIWAXS: The structures were measured using a Xeuss SAXS/WAXS system with Xenocs Genix Cu ULD and Dectris 100 K Pilatus. GIWAXS measurements were performed on the 7.3.3 beamline at the Advanced Light Source (ALS). The 10 keV X-ray beam was incident at a grazing angle of 0.12°–0.15° and selected to maximize the scattering intensity from the samples. Scattered X-rays were detected by using a Dectris Pilatus 2 M photon counting detector. AFM: Surface morphology characterization was performed on a Bruker MultiMode-V AFM in tapping mode, with scanning frequency f = 0.3. TEM: (1) TEM specimen preparation: polymer film-coated SiO₂/Si substrates were dipped into BOE solvent to etch the SiO₂ layer, and then the organic films were transferred onto the water surface and picked up by a copper grid. The residual water was removed by placing the samples into a vacuum chamber overnight. (2) Characterization: A JEOL JEM-2100 TEM, operated at 200 kV, was used to perform dark field imaging and electron diffraction, and a JEOL JEM-2100F TEM, operated at 200 kV, was used to perform high resolution imaging. To suppress the degradation of the organic layer under the electron beam, a cryogenic sample holder was employed to keep the sample at low temperature T = 90 K.