US 2021/0252486 A1Published application

Novel method of manufacture of metal nanoparticles and metal single-atom materials on various substrates and novel compositions

AssigneeThe Curators of the University of Missouri

InventorsXinhua LIANG, Xiaofeng WANG

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Abstract

The present invention discloses a novel method and novel compositions comprising well-dispersed particulate metal materials, including metal nanoparticles and/or metal single-atom materials, on various substrates, said method comprising the use of atomic layer deposition (ALD) and optimization of the metal precursor dose time and the number of ALD cycles. Illustrative of the metals are Fe, Ni, Co, Ru, Rh, Ir, Os, Pt, Pd, and the like; and illustrative of the various substrates are carbon nanotubes (CNTs) (including multi-walled carbon nanotubes (MWCNTs), SiO2, TiO2, alumina, CeO2, ZnO, ZrO2, activated carbon, CuO, Fe2O3, MgO, CaO, graphene, and the like. The density of the dispersed metals on the substrates is significantly higher than the metal density

Claims58

Dependent claims

A method for depositing a metal onto a substrate by using ALD in a suitable reactor, to provide a well-dispersed metal/substrate composition, said method comprising one or more of the following steps:

(a) obtaining a premeasured amount of a suitable metal precursor;
(b) obtaining a premeasured amount of a suitable substrate;
(c) making ready an excess amount of one or more suitable precursor gas;
(d) degassing the substrate at a temperature ranging between about 100° C. and about 200° C. for a period of time ranging between about 5 hours and about 15 hours;
(e) loading the degassed substrate into the reactor;
(f) raising the temperature of the reactor to between about 100° C. and about 500° C.;
(g) fluidizing the substrate particles in the reactor by using flowing inert gas;
(h) loading the metal precursor into a bubbler heated to between about 40° C. and about 280° C.;
(i) carrying the metal precursor particles into the reactor by using flowing inert gas;
(j) feeding the one or more precursor gas separately into the reactor through a distributor plate to react with the metal precursor and produce the metal particles;
(k) subjecting the reactor to vibration from vibrators to enhance particle fluidization during the ALD coating process;
(l) continuing the reaction of the metal precursor and the one or more precursor gas in the reactor for a suitable dose time, and for suitable number of cycles, to result in deposition of the metal particles onto the substrate particles;
(m) flushing the reactor with inert gas to remove unreacted metal precursor and precursor gas and any byproducts;
(n) evacuating and cooling to ambient temperature;
(o) obtaining the well-dispersed metal/substrate composition;
wherein the suitable metal precursor and the one or more precursor gas are selected to be reactive with each other to produce metal particles;
and wherein the suitable reactor is selected from a fluid bed reactor (FBR) or a viscous flow reactor or any other suitable flow types of reactors known in the art;
and wherein said well-dispersed metal/substrate composition comprises metal nanoparticles and/or metal single atoms on said substrate

15 more elements

A composition comprising metal nanoparticles and/or metal single atoms on a substrate, said composition obtained by a novel method for depositing a metal onto a substrate by using ALD in a suitable reactor, wherein said method comprises one or more of the following steps:

(a) obtaining a premeasured amount of a suitable metal precursor;
(b) obtaining a premeasured amount of a suitable substrate;
(c) making ready an excess amount of one or more suitable precursor gas;
(d) degassing the substrate at a temperature ranging between about 100° C. and about 200° C. for a period of time ranging between about 5 hours and about 15 hours;
(e) loading the degassed substrate into the reactor;
(f) raising the temperature of the reactor to between about 100° C. and about 500° C.;
(g) fluidizing the substrate particles in the reactor by using flowing inert gas;
(h) loading the metal precursor into a bubbler heated to between about 40° C. and about 280° C.;
(i) carrying the metal precursor particles into the reactor by using flowing inert gas;
(j) feeding the one or more precursor gas separately into the reactor through a distributor plate to react with the metal precursor and produce the metal particles;
(k) subjecting the reactor to vibration from vibrators to enhance particle fluidization during the ALD coating process;
(l) continuing the reaction of the metal precursor and the one or more precursor gas in the reactor for a suitable dose time, and for suitable number of cycles, to result in deposition of the metal particles onto the substrate particles;
(m) flushing the reactor with inert gas to remove unreacted metal precursor and precursor gas and any byproducts;
(n) evacuating and cooling to ambient temperature;
(o) obtaining the composition comprising metal nanoparticles and/or metal single atoms on the substrate;
wherein the suitable metal precursor and the one or more precursor gas are selected to be reactive with each other to produce metal particles;
and wherein the suitable reactor is selected from a fluid bed reactor (FBR) or a viscous flow reactor or any other suitable flow types of reactors known in the art.

14 more elements

Dependencies are inferred from the claim text.

Facts

Application: 16/972,845Filed 11 Jun 2019
Priority: 22 Jun 2018
Published: 19 Aug 2021
Term ends: Not estimatedThe source records don’t support an estimate.

Classification32 codes

B01J 23/745
Iron group metals: iron
B01J 21/063
Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof: titanium; Oxides or hydroxides thereof
B01J 21/08
Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof: silica
B01J 21/185
Carbon: carbon nanotubes

Family

Application62/688,496Us provisional application · filed 22 Jun 2018
Application62/688,498Us provisional application · filed 22 Jun 2018
US 2021/0252486 A1This patent

From the US filing history. Foreign family members aren’t listed.

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