[특허]Silicon nanosponge particles

Vesta Research, Ltd.

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Silicon nanosponge particles

특허상세정보
국가/구분	United States(US) Patent 등록
국제특허분류(IPC7판)	C01B-033/02 C01B-033/00 B32B-005/32 B32B-005/22
미국특허분류(USC)	423/348; 423/349; 423/350; 428/402
출원번호	UP-0381755 (2006-05-05)
등록번호	US-7569202 (2009-08-24)
발명자 / 주소	Farrell, Declan Limaye, Santosh Y Subramanian, Shanthi
출원인 / 주소	Vesta Research, Ltd.
대리인 / 주소	Bryant, Joy L.
인용정보	피인용 횟수 : 35 인용 특허 : 10

초록

Silicon nanosponge particles prepared from a metallurgical grade silicon powder having an initial particle size ranging from about 1 micron to about 4 microns is presented. Each silicon nanosponge particle has a structure comprising a plurality of nanocrystals with pores disposed between the nanocrystals and throughout the entire nanosponge particle.

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What is claimed is: 1. Silicon nanosponge particles prepared from a metallurgical grade silicon powder having a starting composition consisting of from about 98.6 to about 99.0 weight percent Si; from about 0.03 to about 0.50 weight percent Fe; from about 0.05 to about 0.2 weight percent Al; from about 0.00 to about 0.08 weight percent Ca; from about 0.00 to about 0.15 weight percent C; and from about 0.2 to about 1.0 weight percent O2; wherein the metallurgical grade silicon powder has an initial particle size ranging from about 1 micron to about 4 microns wherein each silicon nanosponge particle comprises a plurality of nanocrystals with nanopores disposed between the nanocrystals and throughout the entire nanosponge particle; wherein each silicon nanosponge particle has a BET surface area of at least about 142 m2/g; and wherein the pores have an average pore diameter ranging from about 2.0 nm to about 8.0 nm as calculated from nitrogen adsorption isotherm data using the Barret-Joyner-Halenda scheme. 2. Silicon nanosponge particles according to claim 1, wherein the silicon nanosponge particles have at least one surface functional group. 3. Silicon nanosponge particles according to claim 2, wherein the surface functional group is selected from the group consisting of: hydrogen, oxygen, halogen, alkenyl, alkyl, organoamine, alkoxy, ester, aldehyde, ketone, carboxylate, and aryl. 4. Silicon nanosponge particles according to claim 1, prepared by: a. providing a metallurgical grade silicon powder having a particle size ranging from about 1 mm to about 3 mm and wherein the metallurgical grade silicon powder has a starting composition consisting of from about 98.6 to about 99.0 weight percent Si; from about 0.03 to about 0.50 weight percent Fe; from about 0.05 to about 0.2 weight percent Al; from about 0.00 to about 0.08 weight percent Ca; from about 0.00 to about 0.15 weight percent C; and from about 0.2 to about 1.0 weight percent O2; b. treating the metallurgical grade silicon powder to yield silicon particles having particle sizes ranging from about 0.1 microns to about 40 microns; c. separating the silicon particles to isolate the silicon particles having sizes ranging from about 1 micron to about 4.0 microns; and d. etching the isolated silicon particles to yield silicon nanosponge particles wherein each silicon nanosponge particle comprises a plurality of nanocrystals with nanopores disposed between the nanocrystals and throughout the entire nanosponge particle; wherein each silicon nanosponge particle has a BET surface area of at least about 142 m2/g; and wherein the pores have an average pore diameter ranging from about 2.0 nm to about 8.0 nm as calculated from nitrogen adsorption isotherm data using the Barret-Joyner-Halenda scheme. 5. Silicon nanosponge particles according to claim 4, wherein the isolated silicon particles are stain etched. 6. Silicon nanosponge particles according to claim 5, wherein the isolated silicon particles are stain etched with a solution comprising HF:HNO3:H2O at a ratio ranging from about 4:1:20 to about 2:1:10 by weight. 7. Silicon nanosponge particles according to claim 6, wherein the nanocrystal size is determined by the concentration of HNO3. 8. Silicon nanosponge particles according to claim 4, wherein the isolated silicon particles are etched by a vapor phase etching process. 9. Silicon nanosponge particles according to claim 8, wherein the vapor phase etching process comprises etching the isolated silicon particles with moist air saturated with HF/HNO3 vapors. 10. Silicon nanosponge particles according to claim 4, further comprising the step of illuminating the isolated silicon particles during etching. 11. Silicon nanosponge particles according to claim 10, wherein illumination occurs at a wavelength selected from the group consisting of: near infrared, visible, near ultraviolet, far ultraviolet, and extreme ultraviolet radiation. 12. Silicon nanosponge particles according to claim 10, further comprising the step of controlling nanocrystal size by illuminating the isolated silicon particles for a determined length of time and controlling the illumination wavelength. 13. Silicon nanosponge particles according to claim 4, further comprising the step of drying the silicon nanosponge particles. 14. Silicon nanosponge particles according to claim 13, wherein the silicon nanosponge particles are dried by a method selected from the group consisting of: air drying; vacuum drying; supercritical drying; freeze drying; and pentane drying. 15. Silicon nanosponge particles according to claim 13, further comprising the step of surface treating the dried silicon nanosponge particles. 16. Silicon nanosponge particles according to claim 15, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at a temperature less than about 300° C. wherein the porous silicon nanosponge particles have an oxygen backbone and a hydrogen terminated surface. 17. Silicon nanosponge particles according to claim 15, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at a temperature of about 300° C. in air wherein surface hydrogen atoms are effused forming a surface mono-layer of oxygen. 18. Silicon nanosponge particles according to claim 15, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at temperatures greater than about 300° C. wherein the porous silicon nanosponge particles undergo oxidation. 19. Silicon nanosponge particles according to claim 18, wherein the dried silicon nanosponge particles are annealed at a temperature of about 900° C. wherein the porous silicon nanosponge particles undergo complete oxidation, forming porous silica. 20. Silicon nanosponge particles according to claim 15, wherein the dried silicon nanosponge particles are surface treated to provide silicon nanosponge particles having at least one surface functional group. 21. Silicon nanosponge particles according to claim 20, wherein the surface functional group is selected from the group consisting of: hydrogen, oxygen, halogen, alkenyl, alkyl, organoamine, alkoxy, ester, aldehyde, ketone, carboxylate, and aryl group. 22. A method for producing silicon nanosponge particles according to claim 1, the method comprising the steps of: a. providing metallurgical grade silicon powder having a particle size ranging from about 1 mm to about 3 mm and wherein the metallurgical grade silicon powder has a starting composition consisting of from about 98.6 to about 99.0 weight percent Si; from about 0.03 to about 0.50 weight percent Fe; from about 0.05 to about 0.2 weight percent Al; from about 0.00 to about 0.08 weight percent Ca; from about 0.00 to about 0.15 weight percent C; and from about 0.2 to about 1.0 weight percent O2; b. treating the silicon powder to yield silicon particles having particle sizes ranging form about 0.1 microns to about 40 microns; c. separating the silicon particles to isolate the silicon particles having a particle size ranging from about 1 micron to about 4 microns; and d. etching the isolated silicon particles to yield silicon nanosponge particles, each silicon nanosponge particle comprising a plurality of nanocrystals with pores disposed between the nanocrystals and throughout the entire silicon nanosponge particle; wherein each silicon nanosponge particle has a BET surface area of at least about 142 m2/g; and wherein the pores have an average pore diameter ranging from about 2.0 nm to about 8.0 nm as calculated from nitrogen adsorption isotherm data using the Barret-Joyner-Halenda scheme. 23. A method according to claim 22, wherein the silicon powder is treated by jet-milling. 24. A method according to claim 22, wherein the isolated silicon particles are stain etched. 25. A method according to claim 24, wherein the isolated silicon particles are stain etched with a solution comprising HF:HNO3:H2O at a ratio ranging from about 4:1:20 to about 2:1:10 by weight. 26. A method according to claim 25, wherein the nanocrystal size is determined by the concentration of HNO3. 27. A method according to claim 22, wherein the isolated silicon particles are vapor phase etched with moist air saturated with HF/HNO3 vapors. 28. A method according to claim 22, further comprising the step of maintaining a constant temperature while etching the isolated silicon particles, wherein the constant temperature is selected from the range from about 0° C. to about 99° C. 29. A method according to claim 22, further comprising the step of illuminating the isolated silicon particles during etching. 30. A method according to claim 29, wherein illumination occurs at a wavelength selected from the group consisting of: near infrared, visible, near ultraviolet, far ultraviolet, and extreme ultraviolet radiation. 31. A method according to claim 29, further comprising the step of controlling nanocrystal size by illuminating the isolated silicon particles for a determined length of time and controlling the illumination wavelength. 32. A method according to claim 22, further comprising the step of etching the porous silicon nanosponge particles with a 50% by weight solution of hydrofluoric acid and ethanol. 33. A method according to claim 22, wherein the silicon nanosponge particles are milled to yield nanocrystalline silicon particles. 34. A method according to claim 22, further comprising the step of drying the silicon nanosponge particles. 35. A method according to claim 34, wherein the silicon nanosponge particles are dried by a method selected from the group consisting of: air drying; vacuum drying, supercritical drying; freeze drying; and pentane drying. 36. A method according to claim 34, further comprising the step of surface treating the dried silicon nanosponge particles. 37. A method according to claim 36, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at a temperature less than about 300° C. wherein the porous silicon nanosponge particles have an oxygen backbone and a hydrogen terminated surface. 38. A method according to claim 36, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at a temperature of about 300° C. in air wherein surface hydrogen atoms are effused forming a surface mono-layer of oxygen. 39. A method according to claim 36, wherein the dried silicon nanosponge particles are surface treated by annealing the dried silicon nanosponge particles at temperatures greater than about 300° C. wherein the porous silicon nanosponge particles undergo oxidation. 40. A method according to claim 39, wherein the dried silicon nanosponge particles are annealed at a temperature of about 900° C. wherein the porous silicon nanosponge particles undergo complete oxidation, forming porous silica. 41. A method according to claim 36, wherein the dried silicon nanosponge particles are surface treated to provide silicon nanosponge particles having at least one surface functional group. 42. A method according to claim 41, wherein the surface functional group is selected from the group consisting of: hydrogen, oxygen, halogen, alkenyl, alkyl, organoamine, alkoxy, ester, aldehyde, ketone, carboxylate, and aryl group. 43. A method for producing silicon nanosponge particles according to claim 1, the method comprising the steps of: a. providing metallurgical grade silicon powder having a particle size ranging from about 1 mm to about 3 mm and wherein the metallurgical grade silicon powder has a starting composition consisting of from about 98.6 to about 99.0 weight percent Si; from about 0.03 to about 0.50 weight percent Fe; from about 0.05 to about 0.2 weight percent Al; from about 0.00 to about 0.08 weight percent Ca; from about 0.00 to about 0.15 weight percent C; and from about 0.2 to about 1.0 weight percent O2; b. jet milling the silicon powder to yield a powder having a particle size ranging from about 0.1 microns to about 40 microns; c. separating the silicon particles to isolate the particles having a particle size ranging from about 1 micron to about 4 microns; and d. stain etching the isolated particles with a solution comprising HF:HNO3:H2O at a ratio ranging from about 4:1:20 to about 2:1:10 by weight to yield silicon nanosponge particles, wherein each silicon nanosponge particle comprises a plurality of nanocrystals with pores disposed between the nanocrystals and throughout the entire silicon nanosponge particle; wherein each silicon nanosponge particle has a BET surface area of at least about 142 m2/g; and wherein the pores have an average pore diameter ranging from about 2.0 nm to about 8.0 nm as calculated from nitrogen adsorption isotherm data using the Barret-Joyner-Halenda scheme.

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