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This study is an attempt to produce gadolinium-doped iron oxide nanoparticles for the purpose of utilization in magnetic fluid hyperthermia (MFH). Six gadolinium-doped iron oxide samples with varying gadolinium contents (<inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mi>G</mi><msub><mi>d</mi><mi>x</mi></msub><mi>F</mi><msub><mi>e</mi><mrow><mn>3</mn><mo>−</mo><mi>x</mi></mrow></msub><msub><mi>O</mi><mn>4</mn></msub><mo>,</mo><mi>x</mi><mo>=</mo><mn>0</mn><mo>,</mo><mo> </mo><mn>0.02</mn><mo>,</mo><mo> </mo><mn>0.04</mn><mo>,</mo><mo> </mo><mn>0.06</mn><mo>,</mo><mo> </mo><mn>0.08</mn><mo>,</mo><mo> </mo><mn>0.1</mn><mo stretchy="false">)</mo></mrow></semantics></math></inline-formula> were prepared using the hydrothermal method <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mi>at</mi><mo> </mo><mn>180</mn><mo> </mo><mo>°</mo><mi mathvariant="normal">C</mi></mrow></semantics></math></inline-formula> and high vapor pressure to incorporate gadolinium ions in the iron oxide structure. The samples were indexed as <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mi>G</mi><mi>d</mi><mi>IO</mi><mo>/</mo><mi>x</mi></mrow></semantics></math></inline-formula>, with <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mi>x</mi></semantics></math></inline-formula> varying from 0.0 to 0.1. The results reveal that gadolinium ions have a low solubility limit in the iron oxide lattice (<i>x</i> = 0.04). The addition of gadolinium caused distortion in the produced maghemite phase and formation of other phases. Based on X-ray diffraction (XRD) analysis and photoelectron spectroscopy (XPS), it was observed that gadolinium mostly crystalized as gadolinium hydroxide, <inline-formula><math xmlns="http://www.w3.org/1998/Math/MathML" display="inline"><semantics><mrow><mi>G</mi><mi>d</mi><mo> </mo><msub><mrow><mrow><mo>(</mo><mrow><mi>O</mi><mi>H</mi></mrow><mo>)</mo></mrow></mrow><mn>3</mn></msub></mrow></semantics></math></inline-formula> for gadolinium concentrations above the solubility limit. The measured magnetization values are consistent with the formed phases. The saturation magnetization values for all gadolinium-doped samples are lower than the undoped sample. The specific absorption rate (SAR) for the pure iron oxide samples was measured. Sample <i>Gd</i>IO/0.04, pure iron oxide doped with gadolinium, showed the highest potential to produce heat at a frequency of 198 kHz. Therefore, the sample is considered to hold great promise as an MFH agent.