# US 9,751,076 B1 · Synthesis of nano crystalline niobia/carbon composites with improved hydrothermal stability

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- Number: US 9,751,076 B1
- Document ID: US9751076B1
- Status: Granted
- Kind: B1
- Application number: 14/094,002
- Filed: 2013-12-02
- Granted: 2017-09-05
- Earliest claimed: 2012-11-30
- Assignees: Stc.Unm
- Applicants: Haifeng Xiong; Abhaya Datye
- Inventors: Haifeng Xiong; Abhaya Datye
- Web page: https://patentgrep.com/patent/US9751076B1

## CPC

- B01J 23/20: Vanadium, niobium or tantalum
- B01J 21/18: Carbon
- B01J 23/6484: {Niobium}
- B01J 35/51: Spheres
- B01J 35/615: {100-500 m2/g}
- B01J 35/633: {less than 0.5 ml/g}
- B01J 35/635: {0.5-1.0 ml/g}
- B01J 37/033: {Using Hydrolysis}
- B01J 37/082: {Decomposition and pyrolysis}
- B01J 35/30: characterised by their physical properties
- B01J 2235/05: Nuclear magnetic resonance [NMR]
- B01J 2235/10: Infrared [IR]
- B01J 2235/15: X-ray diffraction
- B01J 2235/30: Scanning electron microscopy; Transmission electron microscopy
- B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS

## Abstract

Novel transition element-embedded carbon materials and methods for forming the same. The embedded transition elements can be oxides or hydroxides and may include a transition metal. In some cases the transition element-embedded materials are catalytic material suitable for use in a variety of catalytic systems. According to one specific example, the transition element that is embedded is a niobia species.

## Claims

### Claim 1

A method for preparing a transition element carbon composite material comprising:
mixing a compound comprising a transition element with a precipitating agent in a sugar-containing solution at a high enough temperature and for a long enough time that the transition element precipitates to yield a hydroxide and/or oxide while the sugar simultaneously undergoes hydrothermal carbonization; and
heat treating the mixture to form a particulate transition element/carbon material having embedded transition element hydroxide and/or oxide species highly and evenly dispersed through the carbon particles.

### Claim 2 (depends on 1)

The method of claim 1 wherein the transition element is a transition metal.

### Claim 3 (depends on 2)

The method of claim 2 wherein the transition metal is selected from the group consisting of Ag, Au, Ce, Co, Cr, Cu, Fe, Ir, Mn, Mo, Ni, Pt, Ru, Ta, Ti, V, W, and Zr.

### Claim 4 (depends on 2)

The method of claim 2 wherein the transition metal is niobium.

### Claim 5 (depends on 1)

The method of claim 1 wherein the base precipitating agent is urea.

### Claim 6 (depends on 1)

The method of claim 1 wherein the sugar solution is a glucose solution.

### Claim 7 (depends on 1)

The method of claim 1 wherein the high enough temperature is at least 160° C.

### Claim 8 (depends on 7)

The method of claim 7 wherein the high enough temperature is less than 240° C.

### Claim 9 (depends on 1)

The method of claim 1 wherein the long enough time is at least 2 hours.

### Claim 10 (depends on 9)

The method of claim 9 wherein the long enough time is less than 12 hours.

### Claim 11 (depends on 1)

The method of claim 1 wherein the step of heat treatment comprises pyrolysis.

### Claim 12 (depends on 11)

The method of claim 11 wherein pyrolization takes place in an inert atmosphere.

### Claim 13 (depends on 12)

The method of claim 12 wherein pyrolization takes place in a N2 rich atmosphere.

### Claim 14 (depends on 1)

The method of claim 1 wherein the embedded transition element hydroxide and/or oxide species are in the form of discrete transition element hydroxide and/or oxide particles.

### Claim 15 (depends on 14)

The method of claim 14 wherein the discrete transition element hydroxide and/or oxide particles comprise niobium.