To accurately control the freezing rate, a homemade equipment was designed according to a previous report (11). The equipment includes an automatic liquid nitrogen tank, frozen ethanol pool, sample stage (copper cylinder, diameter of 10 cm), and a temperature controller with a heating jacket wrapped the copper cylinder (fig. S4). Ethanol was used as a buffer of the liquid nitrogen due to its low melting point. The temperature controller can show the real-time temperature of the sample stage, maintain steady temperature, and control the freezing rate. Before the sample preparation, the temperature of the sample stage was maintained at −10°C. After adding the solution to the mold, the temperature of the sample stage was controlled to decrease at a constant rate. After the samples were completely frozen, the mold was taken down and the samples were taken out carefully. Note that any possible impact should be avoided, or else cracks will appear on the final samples.

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