北京高压科学研究中心利用自研高压原位核磁装置测试高压下金刚烷的13C NMR谱及压机结构数据集（2023-2025）

高压核磁共振实验在材料科学研究中具有独特价值，但受制于样品腔体积小、内置射频线圈易变形以及信噪比低等问题，仍需寻找更加稳定高效易操作的原位测量方案。本研究北京高压科学研究中心固体核磁平台自主研制了一套外置射频线圈高压原位核磁探头，并在金刚石对顶砧条件下，将金刚烷样品装样至铍铜压机，组装后调谐后在Burker 400MHz 核磁谱仪上进行实验数据采集，在四个压力点下采集金刚烷 13C 谱图，分析信噪比、峰位与展宽随压力变化，谱图经背底扣除与分峰拟合。通过金刚烷的固态 13C NMR 测试验证了装置性能。在 DAC 原位条件下，外置射频线圈布置在上下金刚石压砧之间、样品腔外，有效避免了高压环境对线圈的挤压变形，保证了加载过程中的机械和磁场耦合稳定性，该装置在 0.8–2.2 GPa 范围内可获得比较清晰的 ¹³C 信号，较低压力下信噪比高，压力较高时仍能有较好的分辨能力。桥头碳与非桥头碳两组峰分离度高，便于直接判读与峰分解拟合。该装置在高压核磁测量中表现出结构稳定、趋势可复现的优势，同时也反映出在高压端信噪比和分辨率方面的改进空间。该设计验证了外置线圈方案在高压核磁探测中的可行性和优势，为多核种高压谱学研究提供了新型平台。

High-pressure nuclear magnetic resonance (NMR) experiments hold unique value in materials science research, but are limited by issues such as small sample chamber volume, easy deformation of built-in radio frequency (RF) coils, and low signal-to-noise ratio (SNR), necessitating the exploration of more stable, efficient and easy-to-operate in-situ measurement schemes. In this study, the Solid-State NMR Platform of the Beijing High Pressure Science and Technology Research Center independently developed an external RF coil high-pressure in-situ NMR probe. Under diamond anvil cell (DAC) conditions, adamantane samples were loaded into a beryllium-copper press, and after assembly and tuning, experimental data were collected on a Bruker 400 MHz NMR spectrometer. 13C NMR spectra of adamantane were acquired at four pressure points, and the variations of SNR, peak position and linewidth with pressure were analyzed. The spectra were processed via background subtraction and peak fitting. The performance of the setup was verified through solid-state 13C NMR tests on adamantane. Under DAC in-situ conditions, the external RF coil is placed between the upper and lower diamond anvils, outside the sample chamber, effectively avoiding extrusion deformation of the coil by the high-pressure environment and ensuring mechanical and magnetic coupling stability during the loading process. This setup can obtain relatively clear 13C signals within the pressure range of 0.8–2.2 GPa, exhibiting high SNR at low pressures and maintaining good resolution even at high pressures. The two peaks corresponding to bridgehead and non-bridgehead carbons show high resolution, facilitating direct interpretation and peak decomposition fitting. This setup demonstrates advantages of stable structure and reproducible trends in high-pressure NMR measurements, while also indicating room for improvement in SNR and resolution at high-pressure regimes. This design validates the feasibility and advantages of the external coil scheme for high-pressure NMR detection, providing a novel platform for multi-nuclide high-pressure spectroscopic research.

搜集汇总

背景与挑战

背景概述

该数据集包含北京高压科学研究中心利用自研高压原位核磁装置在0.8–2.2 GPa压力范围内测试的金刚烷13C NMR谱及压机结构数据，验证了外置射频线圈方案在高压核磁探测中的可行性和优势。数据以excel格式储存，适用于高压核磁共振实验的材料科学研究。