US 11,767,605 B1
Preparation method of gradient high-silicon steel by molten salt electrolysis
Zhe Wang, Beijing (CN); Shuqiang Jiao, Beijing (CN); Zheng Huang, Beijing (CN); and Xinrui Wang, Beijing (CN)
Filed by UNIVERSITY OF SCIENCE AND TECHNOLOGY BEIJING, Beijing (CN)
Filed on Jun. 8, 2023, as Appl. No. 18/331,675.
Claims priority of application No. 202310166122.7 (CN), filed on Feb. 27, 2023.
Int. Cl. C25C 7/06 (2006.01); C25C 3/36 (2006.01); C21D 1/84 (2006.01); C21D 1/74 (2006.01); C21D 9/46 (2006.01); C21D 6/00 (2006.01); C22C 38/14 (2006.01); C22C 38/12 (2006.01); C22C 38/06 (2006.01); C22C 38/04 (2006.01); C22C 38/02 (2006.01); C22C 38/00 (2006.01); C25C 7/02 (2006.01)
CPC C25C 7/06 (2013.01) [C21D 1/74 (2013.01); C21D 1/84 (2013.01); C21D 6/005 (2013.01); C21D 6/008 (2013.01); C21D 9/46 (2013.01); C22C 38/001 (2013.01); C22C 38/002 (2013.01); C22C 38/004 (2013.01); C22C 38/008 (2013.01); C22C 38/02 (2013.01); C22C 38/04 (2013.01); C22C 38/06 (2013.01); C22C 38/12 (2013.01); C22C 38/14 (2013.01); C25C 3/36 (2013.01); C25C 7/02 (2013.01); C22C 2202/02 (2013.01)] 7 Claims
OG exemplary drawing
 
1. A preparation method of gradient high-silicon steel by molten salt electrolysis, characterized in that it comprises the following steps:
(1) electrolyte preparation: weighing the inorganic fluoride salt and the inorganic silicon salt, mixing them uniformly and then drying; wherein the molar ratio of the inorganic silicon salt to the inorganic fluoride salt is not more than 1:9, the inorganic silicon salt includes Na2SiF6, K2SiF6, Li2SiF6 or SiO2;
(2) molten salt electrolysis: placing the electrolyte in an electrolysis container, then immersing a cathode and an anode into the electrolyte, heating the electrolysis container to 550° C.-950° C., passing the inert gas through the electrolysis container, and connecting the electrode to the power supply to perform constant current electrolysis, after the electrolysis is finished, the cathode is taken out, washed and dried, wherein the cathode is low silicon steel or pure iron, and the anode is single crystal silicon or polycrystalline silicon, the current density during the electrolysis is 1-20 mA/cm2, and the thickness of the cathode is 0.05 mm-1 mm;
(3) high temperature annealing: placing the dried cathode in a constant temperature region of an annealing furnace; under a protective gas atmosphere, heating the cathode to the target temperature which is 1000-1200° C. at the rate of 5-10° C./min, and maintaining the temperature for a period of time; after the heat treatment, cooling the cathode to the room temperature at the rate of 5-10° C./min ,during which the cathode is always placed in the furnace, and then the gradient high-silicon steel with a uniform silicon concentration difference from the outside to the inside is obtained, wherein the expression of the temperature maintaining time t/min, the target temperature , T′/° C., the thickness of the cathode , x/mm, the difference of the target silicon content in the center of the cathode and the initial silicon content of the cathode, ΔSi/%, and the silicon content gradient k is as follows:

OG Complex Work Unit Math
the expression of the silicon concentration gradient k, the difference between the target silicon content on the surface of the cathode and the target silicon content in the center of the cathode, ΔSt%, and the thickness of the cathode, x/mm is:

OG Complex Work Unit Math
wherein, the target silicon content on the surface of the cathode is not less than 6% and the target silicon content in the center of the cathode is not less than 3%.