Dispersible metal chalcogenide nanoparticles
US-2015118144-A1 · Apr 30, 2015 · US
US10177262B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10177262-B2 |
| Application number | US-201414210012-A |
| Country | US |
| Kind code | B2 |
| Filing date | Mar 13, 2014 |
| Priority date | Mar 15, 2013 |
| Publication date | Jan 8, 2019 |
| Grant date | Jan 8, 2019 |
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Materials and methods for preparing Cu 2 XSnY 4 nanoparticles, wherein X is Zn, Cd, Hg, Ni, Co, Mn or Fe and Y is S or Se, (CXTY) are disclosed herein. The nanoparticles can be used to make layers for use in thin film photovoltaic (PV) cells. The CXTY materials are prepared by a colloidal synthesis in the presence of labile organo-chalcogens. The organo-chalcogens serves as both a chalcogen source for the nanoparticles and as a capping ligand for the nanoparticles.
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We claim: 1. A process for making Cu 2 XSnY 4 nanoparticles, the process comprising: reacting in a solvent a copper precursor, an X precursor and a tin precursor in the presence of a primary chalcogen precursor comprising a labile organo-chalcogen to form a nanoparticle and to form a surface coating on the nanoparticle, the surface coating consisting of the labile organo-chalcogen wherein X is Zn, Cd, Hg, Ni, Co, Mn or Fe and Y is S and/or Se, and wherein the primary chalcogen precursor comprises Se when the X precursor comprises Zn. 2. A process as recited in claim 1 , wherein the copper precursor is an acetate, an acetylacetonate or a chloride. 3. A process as recited in claim 1 , wherein the X precursor is an acetate, an acetylacetonate, a chloride or a stearate. 4. A process as recited in claim 1 , wherein the X precursor is zinc(II) acetate. 5. A process as recited in claim 1 , wherein the X precursor is cadmium(II) acetate. 6. A process as recited in claim 1 , wherein the X precursor is iron(II) acetylacetonate. 7. A process as recited in claim 1 , wherein the X precursor is iron(III) acetylacetonate. 8. A process as recited in claim 1 , wherein the tin precursor is a chloride. 9. A process as recited in claim 1 , wherein the solvent is dichloromethane. 10. A process as recited in claim 1 , wherein the tin precursor is tin(IV) acetate, tin(IV) bis(acetylacetonate) dichloride, or triphenyl(trimethyl) tin. 11. A process as recited in claim 1 , wherein the solvent is a non-coordinating solvent. 12. A process as recited in claim 1 , wherein the solvent is 1-octadecene or a heat transfer fluid. 13. A process as recited in claim 1 , wherein reacting comprises mixing the copper precursor, X precursor, tin precursor and labile organo-chalcogen in a solvent at a first temperature not greater than 50° C. and then heating the solvent to a second temperature for a first time interval. 14. A process as recited in claim 13 , wherein the first time interval is about 1 hour. 15. A process as recited in claim 1 , wherein the second temperature is between 180° C. and 300° C. 16. A process as recited in claim 1 , wherein the second temperature is between 220° C. and 240° C. 17. A process as recited in claim 1 , wherein the labile organo-chalcogen comprises 1-octanethiol, 1-dodecanethiol, t-dodecanethiol, 2-naphthalenethiol, 1-octane selenol or 1-dodecane selenol. 18. A process as recited in claim 1 , further comprising the addition of a secondary chalcogen precursor. 19. A process as recited in claim 18 , wherein the secondary chalcogen precursor is trioctylphosphine sulphide or trioctylphosphine selenide. 20. A process as recited in claim 1 , wherein reacting comprises mixing the copper precursor, X precursor, tin precursor and labile organo-chalcogen in a solvent at a first temperature not greater than 50° C. to form a mixture, heating the mixture to a second temperature to remove the solvent, and heating the remainder of the mixture to a third temperature.
Compounds containing, besides selenium or tellurium, more than one other element, with -O- and -OH not being considered as anions · CPC title
organic substances {(organic macromolecular compounds or compositions C08)} · CPC title
mainly consisting of other non-metallic substances · CPC title
Compounds containing tin, with or without oxygen or hydrogen, and containing two or more other elements · CPC title
by thermal analysis data, e.g. TGA, DTA, DSC · CPC title
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