使用聚二甲基硅氧烷（PDMS）胶带，通过机械去角质对MOS2，MOSE2，WS2和WSE2（HQ石墨烯）（HQ石墨烯）剥落。
这项研究的气密细胞分为两个部分：作为化学储层和带有光学窗口的底板。储层的体积约为2 mL，足以监测缓慢的反应动态几天，以避免蒸发的任何问题。储层部分的两个端口与管子连接到注射器。第一个注射器是通过填充大约3毫升n-buli（在己烷中1.6 m，sigma-aldrich）来制备的，当将化学物质注入细胞内部时，将第二个空注射器作为排气容器（氮）制备。带有TMD薄片的玻璃基板，带有两个注射器的细胞的两个部分和一个O形圈（直径1.8毫米，EL-Cell）组装在氮杂物箱中。该单元格在定制的RICM上。定位所需的薄片后，我们对N-Buli注射了大约1分钟，导致注射器2的部分填充。去角质片的顶侧与N-Buli接触。底部接触在RICM测量过程中观察到薄片的玻璃基板。仔细监测了两个注射器中的N-Buli水平，以确保在实验过程中保持完全浸入。
我们注意到，据报道，均扭曲了1T'相和1T期的共验证2,25,28,29,42,44。但是，这两个阶段在光学分辨率上是无法区分的，在整个研究中，我们将1T'/1T相表示为1T。2H-TMD的静态形式形成1T-溶解度，在空气中稳定2,25。为了去除多余的丁锂和其他有机副产物44，我们首先使用过量的N-己烷洗涤了样品。洗涤步骤是通过使用注射器注入N-己烷在细胞内完成的，以避免空气暴露并最大程度地减少表面可能氧化的机会。在稳态光学表征（光致发光和拉曼）之后，我们使用过量的蒸馏水（DI），丙酮和异丙醇（IPA）再次冲洗样品，以去除所有锂（1T-TMDS）。
使用Renishaw Invia Raman显微镜在环境条件下使用激发激光源在环境条件下进行显微镜稳态光致发光和拉曼测量。在所有测量值之前，使用硅参考样品校正仪器响应来校准光谱仪。激光设置为0.05％（<0.5 µW) focused on the designated point of the flake using a 100× long working distance objective (numerical aperture = 0.85), and the emission was collected in streamline mode and dispersed by 1,800 l mm−1 grating.
Reflection microscopy was performed with a custom-built microscope. A variable wavelength excitation was provided by a pulsed super-continuum white light source (Fianium Whitelaser) coupled to a monochromator (Bentham TMC 300). The sample was imaged, at each wavelength, in reflection geometry onto an EMCCD camera (Photometrics QuantEM 512SC) with a 60× oil immersion objective (UPLFLN60XOI, Olympus). The microscopic photoluminescence image was taken on the same setup, using 532 nm excitation and imaging onto the EMCCD camera with a 660-nm bandpass filter (Thorlabs).
RICM measurements were carried out using a custom-built microscope setup reported in detail previously32,44. Furthermore, the microscope was equipped with a 455-nm LED (M455L4, Thorlabs) coupled into a single-mode fibre. The output of the fibre was collimated with a condenser lens and imaged into the back focal plane of the objective (UPLXAPO100XO, Olympus) to achieve wide-field illumination. The 730 nm illumination was carried out by inserting a 730-nm bandpass filter (FB730-10, Thorlabs) into the illumination path of a SOLIS-740C (Thorlabs). The magnification of the microscope was 167× and confirmed with a resolution target. A 2 × 2 software-based pixel binning, leading to a pixel pitch of approximately 70 nm per pixel, and, depending on the experiment, 10–30 frame binning was applied to improve the image quality. The effective acquisition frame rates varied between 0.05 Hz (730 nm illumination) and 3 Hz (455 nm illumination, 510 mW cm−2) ensuring sufficient time resolution to monitor the phase transformation dynamics.
Throughout the experiment, the sample was kept in focus using a hardware-based autofocus routine32. No images were recorded during the injection of n-BuLi because of the large pressure fluctuations and associated focus changes of the sample. For the patterning experiments (Fig. 3a), a shadow mask was placed into the illumination path of the microscope such that it was imaged onto the sample. The flake was carefully positioned with respect to the mask in the absence of n-BuLi. Subsequently, the illumination was turned off and n-BuLi was injected as before. After 1 min, the syringe pump was turned off and the 455 nm illumination was switched on to initiate the photo-driven phase transition. The light source was turned off once the intensity of the flake was reduced to the 1T phase value, and the sample was washed immediately afterwards.
Recorded image stacks were corrected for sample drift as previously described32. No other post-processing was applied.
For the histogram analysis presented in Fig. 2, the image stack was masked to include only 1L or 2L regions. The first image in each stack served as a reference frame to compute an average intensity value for each masked region. For each image in the stack, each pixel value in the masked image was subsequently divided by this reference intensity value to generate an intensity distribution centred at 1 (the mean intensity of the first image is computed and used to normalize all subsequent intensity histograms). For each image in the stack, a histogram with 120 equally spaced bins ranging from intensity values of 0.1–1.2 was then computed, yielding the histogram plots shown in Fig. 2. Generally, no normalization for the illumination intensity was required because of the high stability of the LED light sources (<5% power drop over 5 days continuous illumination). The intensity histogram is in the first instance a convolution of the actual intensity value and the noise characteristics of the camera. We verified shot-noise limited performance and can conclude that the noise broadening is well below 1%, causing no notable broadening of the normalized histograms.
During long-term experiments (>1 h），对于捕获730 nm照明下的相变动力学所需的必要条件，我们观察到在12小时内，玻璃/n-buli界面的强度的明显变化高达15％。这些变化与图2b，c中观察到的长期增加相匹配，因此必须相关。鉴于我们的光源是稳定的，因此这种行为的起源必须与N-Buli溶液的折射率的变化或增加的异常散射机制有关。
除了这种缓慢的强度增加外，在730 nm处的长期成像显示了几个类似聚类的颗粒的几个着陆事件。这些颗粒可能是在涉及高反应性n-布利的溶液反应中形成的。因此，我们认为，反射强度的长期增加很可能与聚焦外散射有关，我们的宽场显微镜将对它们敏感。
在2032型电池中进行了散装过渡金属二分法作为工作电极的电化学性能。通过将80％活性材料，10 wt％的导电剂（Super-P）和10 wt％粘合剂（聚偏二氟化物）铸造在N-甲基-2-吡咯烷酮上的浆液中，制造了工作电极。然后将涂层的电极在真空中在50°C下干燥过夜。将测试电池组装在一个充满氩气的手套箱（<0.5 ppm的氧和水）中，锂芯片切成圆形（直径16 mm）作为反电极，多孔聚丙烯分离剂（Celgard 2400）（celgard 2400）和1 m lipf6在乙烯碳酸盐/二乙二烯碳酸盐/二乙二醇（V/V/V）中，均为V/v/v/v/v/v/v/v/v/v/v。电解质。活性材料的质量负载约为1-1.5 mg cm -2。在室温下老化20小时后，这些细胞准备好进行详细的电化学测试。根据每种活性材料在0.01–2.8 V. 0.01–2.8 V. 0.01–2.8 V的理论能力下，以0.01-2.8 V的理论能力以0.1 mV s -1的速率在潜在的LI+0.01 -180 -01 -180范围内，以0.1 mV的速率进行了旋转电池测试测试。
通过使用阴影面膜通过金属沉积制造光电探测器。使用电子束蒸发（PVD 200 Pro，Kurt J. Lesker）选择性地将黄金垫（50 nm）选择性地沉积在1T/1T'区域上。通过通过定制的镜头（Mitutoyo）照亮单色激光器（MCLS1，Thorlabs），并使用半导体分析仪（Keithley 4200）记录光电流，从而进行光电探测器测量。
