1：Experimental Design and Method Selection:

Hybrid nanoparticles were prepared using a phase-separated film shattering process with varying iron oxide concentrations while keeping a fixed ratio of conjugated polymer and phospholipid. Structural and property analyses were conducted using techniques like X-ray diffraction and transient absorption spectroscopy.

2：Sample Selection and Data Sources:

Samples included PCPDTBT, D8PE, and Fe3O4 nanoparticles at molar mixing ratios from 1:1:0 to 1:1:1. Data were sourced from synthesized nanoparticles and characterized using various instruments.

3：Data were sourced from synthesized nanoparticles and characterized using various instruments. List of Experimental Equipment and Materials:

3. List of Experimental Equipment and Materials: Materials included PCPDTBT, D8PE, Fe3O4 nanoparticles, octanoic acid, PEG-NHS, chloroform, and others. Equipment included ultrasonicator, UV-vis-NIR spectrometer, TEM, DLS, MRI scanner, synchrotron X-ray scattering setup, and femtosecond transient absorption spectrometer.

4：Experimental Procedures and Operational Workflow:

Films were prepared by dissolving materials in chloroform, evaporating solvent, annealing, and shattering with water under ultrasonication. Nanoparticles were characterized for size, absorption, PA intensity, T2 relaxation, and structure via X-ray scattering and TA spectroscopy.

5：Data Analysis Methods:

Data were analyzed using software for DLS, TEM image analysis, spectral fitting, and multi-exponential decay fitting for TA data.