US 12,214,336 B2
Metal-free few-layer phosphorous nanomaterial: method for its preparation and use thereof
Qingzhe Zhang, Longueuil (CA); Dongling Ma, Pointe-Claire (CA); and Mohamed Chaker, Montreal (CA)
Assigned to INSTITUT NATIONAL DE LA RECHERCHE SCIENTIFIQUE, Quebec (CA)
Filed by INSTITUT NATIONAL DE LA RECHERCHE SCIENTIFIQUE, Quebec (CA)
Filed on Feb. 15, 2024, as Appl. No. 18/442,745.
Application 18/442,745 is a division of application No. 17/045,570, abandoned, previously published as PCT/CA2019/050813, filed on Jun. 10, 2019.
Claims priority of provisional application 62/685,371, filed on Jun. 15, 2018.
Prior Publication US 2024/0307857 A1, Sep. 19, 2024
Int. Cl. B01J 27/00 (2006.01); B01J 27/14 (2006.01); B01J 27/24 (2006.01); B01J 35/39 (2024.01); B01J 37/00 (2006.01); B01J 37/04 (2006.01); B01J 37/06 (2006.01); C01B 3/04 (2006.01); C01B 25/02 (2006.01)
CPC B01J 27/14 (2013.01) [B01J 27/24 (2013.01); B01J 35/39 (2024.01); B01J 37/0072 (2013.01); B01J 37/009 (2013.01); B01J 37/04 (2013.01); B01J 37/06 (2013.01); C01B 3/042 (2013.01); C01B 25/02 (2013.01); C01P 2002/72 (2013.01); C01P 2004/24 (2013.01)] 15 Claims
OG exemplary drawing
 
1. A method for preparing a few-layer phosphorous nanomaterial, comprising:
(a) providing a bulk layer-structured phosphorous material;
(b) grinding the bulk phosphorous material;
(c) dispersing the grinded material into a first organic solvent to obtain a first dispersion in a sealed vial;
(d) freezing the first dispersion for a period of time using liquid nitrogen, wherein organic solvent molecules are intercalated between layers of the material and interlayers are expanded;
(e) melting the frozen dispersion via ultrasonication for a period of time to obtain a second dispersion, wherein forces are generated between intercalated organic ice crystals and the layers; and
(f) submitting the second dispersion to a separation step, optionally involving centrifugation for a period of time, to obtain the nanomaterial,
wherein the first organic solvent is selected from the group consisting of N-methyl-2-pyrrolidone (NMP), diethyl ether, chloroform, tetrahydrofuran, cyclohexane, toluene, dimethylformamide, and combinations thereof,
and wherein the method is conducted in a glovebox or with nitrogen bubbling.