SiP crystal growth regulation and control method
A crystal growth and crystal technology, which is applied in the field of SiP crystal growth regulation, can solve the problems of high reaction temperature and long time, and achieve the effect of simple and mature process, high output and high yield
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[0022] The preparation method of a kind of SiP crystal material provided by the present invention comprises as follows:
[0023] (1) Weigh a certain proportion of silicon source, phosphorus source, transport agent, regulator in the glove box, fully mix and transfer to the quartz tube;
[0024] (2) Vacuumize and seal the quartz tube, and sinter at high temperature in a heating device for a certain period of time;
[0025] (3) Wash with solvent after cooling, and obtain the material after vacuum drying.
[0026] In the above steps, the molar ratio of Si in the silicon source, P in the phosphorus source, the transport agent, and the regulating agent in step (1) is 1:1:(0.005-0.5):(0.01-0.1);
[0027] The silicon source is one or a combination of crystalline silicon, amorphous silicon, and silicon tetraiodide;
[0028] The phosphorus source is one or a combination of red phosphorus, yellow phosphorus, white phosphorus, fiber phosphorus, purple phosphorus and phosphorus triiodide...
Embodiment 1
[0036] Weigh 0.14g of amorphous silicon powder, 0.16g of red phosphorus powder, 15.9mg of tellurium tetraiodide, and 1.6mg of S powder in a glove box. The raw materials are fully ground and evenly added to a quartz tube with a length of 11cm and an inner diameter of 11mm. Seal the quartz tube with an oxyhydrogen machine after vacuum. Put the sealed quartz tube in a box furnace, set the furnace temperature to 1200°C, and the reaction time is 12 hours. After the furnace cools down, take out the SiP linear crystal, clean it with acetone and ethanol, and dry it in vacuum. Finally, the SiP linear crystal The yield was 92%. Crystal XRD (a) and Raman spectrum (b) as figure 1 shown. SEM (a) and SEM Mapping (b) of SiP crystal as figure 2 shown. SiP linear crystal photography picture as image 3 shown.
[0037] figure 1 XRD of a and figure 1 The Raman result of b shows that the obtained is indeed SiP, and the XRD peak shape is sharp and the peak intensity is very high, indicati...
Embodiment 2
[0039] Weigh 0.28g of crystalline silicon powder, 0.31g of fiber phosphorus, 1.275g of iodine element, and 79mg of elemental selenium in the glove box. The raw materials are fully ground and evenly added to a quartz tube with a length of 25cm and an inner diameter of 16mm. The oxygen machine seals the quartz tube. Put the sealed quartz tube in a muffle furnace at a temperature of 900°C and a reaction time of 680 hours. After the furnace cools down, take out the SiP linear crystals, clean them with acetone and ethanol, and dry them in vacuum. The final yield of SiP linear crystals is 95%.
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