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1. (WO2017189509) TRANSITION METAL CATALYST NANOPARTICLES AND USES THEREOF
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CLAIMS

A microparticle comprising carbon and a plurality of nanoparticles comprising one or more transition metal compounds selected from the group consisting of transition metal carbides, transition metal nitrides, transition metal sulfides, transition metal phosphides, transition metal carbonitrides, transition metal sulfonitrides, transition metal carbosulfides, transition metal phosphocarbides, transition metal phosphonitrides, transition metal phosphosulfides, transition metal carbosulfonitrides, transition metal carbophosphonitrides, transition metal phosphosulfonitrides, transition metal carbophosphosulfonitrides, and interstitial derivatives thereof, wherein the plurality of nanoparticles are supported on the surface of the microparticle.

The microparticle of claim 1, wherein the microparticle further comprises one or more transition metals.

The microparticle of claims 1 and 2, wherein the one or more transition metals are selected from the group consisting of tungsten, nickel, iron, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, palladium, and platinum. The microparticle of claims 1-3, wherein the microparticle is substantially spherical. The microparticle of claims 1-4, wherein average particle size of the microparticle is 30 μΜ or less.

The microparticle of claims 1-5, wherein average particle size of the microparticle is 10 μΜ or less.

The microparticle of claims 1-6, wherein the microparticle is substantially spherical and has a diameter in the range of from 1.5 μΜ to 10 μΜ.

The microparticle of claims 1-7, wherein the microparticle has a diameter in the range of from 3 μΜ to 5 μΜ.

The microparticle of claims 1-8, wherein the surface of the microparticle is smooth and the plurality of nanoparticles are substantially uniformly dispersed over the surface of the microparticle.

10. The microparticle of claims 1-9, wherein the average particle size of the nanoparticles is 5 nM or less.

11. The microparticle of claims 1-10, wherein the average particle size of the

nanoparticles is in the range of from 3 nM to 5 nM.

12. The microparticle of claims 1-11, wherein the transition metal of the one or more transition metal compounds is selected from the group consisting of tungsten, nickel, iron, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, palladium, platinum, and combinations thereof.

13. The microparticle of claims 1-12, wherein the nanoparticles comprise tungsten carbide.

14. The microparticle of claims 1-13, wherein the interstitial derivative comprises one or more transition metals selected from the group consisting of tungsten, nickel, iron, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, platinum, and palladium.

15. The microparticle of claims 1-14, wherein the nanoparticles have a core/shell structure.

16. A membrane comprising a plurality of microparticles in accordance with claims 1- 15, wherein the transition metal of the transition metal compound is selected from the group consisting of tungsten, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, and combinations thereof.

17. The membrane of claim 16, wherein the membrane comprises an ionomer.

18. The membrane of claims 16 and 17, wherein the ionomer comprises one or more functional groups selected from the group consisting of sulfonic acid/sulfonate groups, phosphonic acid/phosphonate groups, and carboxylic acid/carboxylate groups.

19. The membrane of claims 16-18, wherein the membrane comprises a

poly(perfluorosulfonic acid).

20. The membrane of claims 16-19, wherein the poly(perfluorosulfonic acid) is a tetrafluoroethylene-based copolymer.

21. The membrane of claims 16-20, wherein the membrane further comprises one or more transition metals selected from the group consisting of tungsten, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, platinum, and palladium.

22. The membrane of claims 16-21, wherein the nanoparticles comprise tungsten carbide.

23. The membrane of claims 16-22, wherein the microparticles are present in the membrane in a concentration in the range of from 1 % to 10 % by weight, based on the total weight of the membrane.

24. The membrane of claims 16-23, wherein the microparticles are uniformly

distributed throughout the membrane.

25. The membrane of claims 16-24, wherein the concentration of the microparticles in the membrane varies transversely across the membrane.

26. The membrane of claims 16-25, wherein the concentration of the microparticles in the membrane increases or decreases in a gradient transversely across the membrane.

27. The membrane of claims 16-26, wherein the membrane has a thickness in the range of from 10 μΜ to 100 μΜ.

28. The membrane of claims 16-27, wherein the membrane has a thickness in the range of from 15 μΜ to 25 μΜ.

29. The membrane of claims 16-28, wherein the membrane is reinforced.

30. The membrane of claims 16-29, wherein the membrane is reinforced with

polytetrafluoroethylene and/or carbon nanotubes.

31. The membrane of claims 16-30, wherein the reinforcement is located in the center of the membrane or closer to one surface of the membrane relative to the other surface of the membrane.

32. A process for preparing a microparticle comprising carbon and a plurality of

nanoparticles comprising one or more transition metal compounds selected from the group consisting of transition metal carbides, transition metal nitrides, transition metal sulfides, transition metal phosphides, transition metal

carbonitrides, transition metal sulfonitrides, transition metal carbosulfides, transition metal phosphocarbides, transition metal phosphonitrides, transition metal phosphosulfides, transition metal carbosulfonitrides, transition metal carbophosphonitrides, transition metal phosphosulfonitrides, and transition metal carbophosphosulfonitrides, comprising the steps of:

(a) subjecting a mixture of (1) one or more precursors comprising a transition metal and (2) a precursor comprising carbon to hydrothermal carbonization to form an intermediate; and

(b) subjecting the intermediate formed in (a) to temperature- programmed reduction-carburization, temperature-programmed reduction-nitridation, a temperature-programmed reduction- sulfidation and/or a temperature-programmed reduction- phosphidation to form a microparticle comprising carbon and a plurality of nanoparticles comprising a transition metal carbide, transition metal nitride, transition metal sulfide, transition metal phosphide, transition metal carbonitride, transition metal sulfonitride, transition metal carbosulfide, transition metal phosphocarbide, transition metal phosphonitride, transition metal phosphosulfide, transition metal carbosulfonitride, transition metal carbophosphonitride, transition metal phosphosulfonitride, and/or transition metal carbophosphosulfonitride.

33. The process of claim 32, wherein the process forms a microparticle comprising carbon wherein the plurality of nanoparticles are supported on the surface of the microparticle.

34. The process of claims 32 and 33, wherein the transition metal of the precursor comprising a transition metal is selected from the group consisting of tungsten, nickel, iron, cobalt, molybdenum, rhodium, iridium, zinc, copper manganese, chromium, platinum, palladium, and combinations thereof.

35. The process of claims 32-34, wherein the precursor comprising a transition metal comprises ammonium metatungstate hydrate.

The process of claims 32-35, wherein the precursor comprising carbon is a water-soluble carbohydrate obtained from food and/or lignocellulosic biomass.

The process of claims 32-36, wherein the precursor comprising carbon is selected from the group consisting of C5 and C6 sugars and their oligomers.

The process of claims 32-37, wherein the precursor comprising carbon is selected from the group consisting of glucose, sucrose, fructose, galactose, and

combinations thereof.

The process of claims 32-38, further comprising ball milling the intermediate formed in step (a) prior to step (b).

The process of claims 32-39, further comprising post-treatment of the microparticle formed in (b) to form an interstitial derivative of the transition metal carbide, transition metal nitride, transition metal sulfide, transition metal phosphide, transition metal carbonitride, transition metal sulfonitride, transition metal carbosulfide, transition metal phosphocarbide, transition metal phosphonitride, transition metal phosphosulfide, transition metal carbosulfonitride, transition metal carbophosphonitride, transition metal phosphosulfonitride, and/or transition metal carbophosphosulfonitride.

The process of claim 40, wherein the post-treatment is selected from the group consisting of atomic layer deposition and colloidal synthesis.

The process of claims 32-41, wherein the interstitial derivative comprises one or more transition metals selected from the group consisting of tungsten, nickel, iron, cobalt, molybdenum, rhodium, iridium, zinc, copper, manganese, chromium, platinum, and palladium.

A fuel cell comprising an anode, a cathode, an anode catalyst, and a membrane in accordance with claims 16-31.