US11306002B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-11306002-B2 |
| Application number | US-201716491741-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 7, 2017 |
| Priority date | Mar 7, 2017 |
| Publication date | Apr 19, 2022 |
| Grant date | Apr 19, 2022 |
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The present invention relates to a process for the synthesis of a composite material comprising steps of: (a) reacting gaseous magnesium (Mg) and silica (SiO 2 ) in an inert atmosphere; (b) washing the product obtained in step (a) in an acidic medium; and (c) reacting further gaseous magnesium (Mg) with the silica (SiO 2 ) and silicon (Si) product obtained in step (b). The process of the invention allows Mg 2 Si/MgO nanocomposites to be prepared without too many separate steps, and wherein the MgO phase is homogeneously dispersed within the Mg 2 Si matrix. The nanocomposites obtained may for example find practical application as thermoelectric materials in thermoelectric generators.
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The invention claimed is: 1. A process for the synthesis of a composite material comprising the steps of: (a) reacting gaseous magnesium (Mg) and silica (SiO 2 ) at a temperature of at least 500° C. and at most 1200° C. in an inert atmosphere; (b) washing the product obtained in step (a) in an acidic medium until neutralization is achieved to obtain a product containing the silica (SiO 2 ) and silicon (Si); and (c) reacting further gaseous magnesium (Mg) with the product obtained in step (b) at a temperature of at least 500° C. and at most 1200° C. in an inert atmosphere. 2. The process according to claim 1 , wherein the silica (SiO 2 ) used in step (a) consists of cylindrical slices with 5 to 20 mm in diameter and 1 to 5 mm in height. 3. The process according to claim 1 , wherein the silica (SiO 2 ) used in step (a) consists of silica particles having size ranges of 100 nm to 1000 nm and porosities of 70 to 95%. 4. The process according to claim 1 , wherein the molar ratio of Mg:SiO 2 in step (a) is at least 0.5 and at most 2. 5. The process according to claim 1 , wherein in step (a), the maximum temperature reached is at least 500° C. and at most 1200° C. 6. The process according to claim 1 , wherein the duration of step (a) is at least 30 min and at most 5 hrs. 7. The process according to claim 1 , wherein in step (a), the maximum temperature is reached by heating from room temperature to the maximum temperature at a rate of at 1-30° C./min. 8. The process according to claim 1 , wherein in step (b), the acidic medium consists of aqueous HCl. 9. The process according to claim 1 , wherein for step (c), the molar ratio of Mg:SiO 2 is at least 2 and at most 8. 10. The process according to claim 1 , wherein the maximum temperature for step (c) is at least 500° C. and at most 1200° C. 11. The process according to claim 1 , wherein the duration of step (c) is at least 30 min and at most 5 hrs. 12. The process according to claim 1 , wherein, the maximum temperature is reached by heating from room temperature at a rate of at least 0.5° C./min and at most 10° C./min in step (c). 13. The process according to claim 1 , wherein the inert atmosphere in step (a) and/or step (c) contains at least one of the following: nitrogen (N 2 ), argon (Ar). 14. The process according to claim 7 , wherein the rate is 10-30° C./min. 15. The process according to claim 10 , wherein the maximum temperature is at least 600° C. and at most 800° C. 16. The process according to claim 13 , wherein the inert atmosphere is at least argon. 17. The process according to claim 1 , wherein in step (a) and step (b), the maximum temperature is at least 600° C. and at most 800° C.
mainly consisting of other non-metallic substances · CPC title
obtained by TEM, STEM, STM or AFM · CPC title
by d-values or two theta-values, e.g. as X-ray diagram · CPC title
by reduction of silica or {free} silica-containing material · CPC title
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