Microwave and Laser Assisted Production Refractory Metal Oxides

This application claims the benefit of U.S. Provisional Patent Application No. 63/571,840, filed Mar. 29, 2024, the entire contents of which are hereby incorporated by reference for all purposes in its entirety.

Transition metal dichalcogenides (TMDs) are atomically thin and layered semiconductors formed of transition metals and chalcogen atoms. Examples of the transition metals include molybdenum and tungsten and examples of the chalcogen atoms include sulfur and selenium. TMD examples include molybdenum disulfide, tungsten disulfide, and their selenides. TMDs have been used in several applications in energy generation and energy storage. Examples include in solar cells and in batteries. Additionally, their 2 forms, having fewer layers of sheets, have drawn interest recently.

TMDs, however, do have drawbacks. The state-of-the-art method of producing TMOs is from the ores of these metals found in the earth's crust. Most of these refractory metals are found in the form of sulfides in the earth's crust. These sulfide ores are heated in furnaces at temperatures in the upwards of 800-1000° C. in a process called roasting. TMDs are difficult to synthesize on a large scale, have high contact resistance, and are susceptible to environmental degradation. There are also challenges in using TMDs to achieve consistent performance due to variations in material quality.

Therefore, there is a need for a material to use in energy generation and energy storage that has improved synthesis and performance compared to TMDs.

Covered embodiments of the present disclosure are defined by the claims, not this summary. This summary is a high-level overview of various aspects of the invention and introduces some of the concepts that are further described in the Detailed Description section below. This summary is not intended to identify key or essential features of the claimed subject matter, nor is it intended to be used in isolation to determine the scope of the claimed subject matter. The subject matter should be understood by reference to appropriate portions of the entire specification, any or all drawings and each claim.

In some aspects, the present disclosure is directed to a method for generating a crystalline transition metal oxide. The method may comprise: receiving a transition metal ore; and generating a crystalline transition metal oxide corresponding to the transition metal ore by applying a microwave power or a laser power to the transition metal ore. In some aspects, the method may comprise applying the microwave power. In some aspects, the method may comprise applying the laser power. The microwave power may be provided at a power from 500 to 1200 W or from 700 to 900 W. The laser power may be provided at a power from 1 to 100W. The laser power may be a blue light with a wavelength from 380 to 500 nm. The transition metal ore may have a formula of MX, wherein M is a transition metal atom and X is a chalcogen atom. In some aspects, M is Mn, Mo, Cr, Ti, V, Zr, Nb, Tc, Ta, Hf, W, or Re. In some aspects, X is Se, S, or Te. In some aspects, the transition metal ore is MoSe, MoS, WSc, WS, MoTe, or combinations thereof. In some aspects, the transition metal ore is MoS. When the transition metal ore is MoS, the crystalline transition metal oxide may be primarily alpha-MoO. In some aspects, the crystalline transition metal oxide comprises layered crystals, such as layered crystals having a size of at least 1 micron in length. In some aspects, the crystalline transition metal oxide comprises microbelts, such as microbelts having a size of at least 500 micron in length. In some aspects, the crystalline transition metal oxide has less than 5 ppm impurities.

In some aspects, the present disclosure is directed to a method for generating a crystalline MoO. The method may comprise receiving MoS2; and generating crystalline MoOby applying a microwave power or a laser power to the MoS2; wherein the MoOis primarily alpha-MoO3.In some aspects, at least 80% of the MoO3 is alpha-MoO3. In some aspects, the method may comprise applying the microwave power. In some aspects, the method may comprise applying the laser power. The microwave power may be provided at a power from 500to 1200 W or from 700 to 900 W. The laser power may be provided at a power from 1 to 100 W. The laser power may be a blue light with a wavelength from 380 to 500 nm. In some aspects, the crystalline MoOcomprises layered crystals, such as layered crystals having a size of at least 1 micron in length. In some aspects, the crystalline MoOcomprises microbelts, such as microbelts having a size of at least 500 micron in length. In some aspects, the MoOhas less than 5 ppm impurities.

Further aspects, objects, and advantages will become apparent upon consideration of the detailed description.

Before the present disclosure is described in detail, it is to be understood that the terminology used herein is for purposes of describing particular examples and embodiments only, and is not intended to be limiting.

In this specification and in the claims that follow, reference will be made to a number of terms that shall be defined to have the following meanings:

As used herein, the terms “optional” or “optionally” as used herein mean that the subsequently described feature or structure may or may not be present, or that the subsequently described event or circumstance may or may not occur, and that the description includes instances where a particular feature or structure is present and instances where the feature or structure is absent, or instances where the event or circumstance occurs and instances where it does not.

Where a range of values is provided, it is understood that each intervening value, to the tenth of the unit of the lower limit unless the context clearly dictates otherwise, between the upper and lower limits of that range is also specifically disclosed. Each smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in that stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range, and each range where either, neither or both limits are included in the smaller ranges is also encompassed within the invention, subject to any specifically excluded limit in the stated range. Where the stated range includes one or both of the limits, ranges excluding either or both of those included limits are also included in the invention.

As used herein, “comprising” is synonymous with “including,” “containing,” or “characterized by,” and is inclusive or open-ended and does not exclude additional, unrecited elements or method steps. As used herein, “consisting of” excludes any element, step, or ingredient not specified in the claim element. As used herein, “consisting essentially of” does not exclude materials or steps that do not materially affect the basic and novel characteristics of the claim. Any recitation herein of the term “comprising”, particularly in a description of components of a composition, in a description of a method, or in a description of elements of a device, is understood to encompass those compositions, methods, or devices consisting essentially of and consisting of the recited components or elements, optionally in addition to other components or elements. The invention illustratively described herein suitably may be practiced in the absence of any element, elements, limitation, or limitations which is not specifically disclosed herein.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention, the preferred methods and materials are now described. All publications mentioned herein are incorporated herein by reference to disclose and describe the methods and/or materials in connection with which the publications are cited.

The present disclosure is directed to a method of producing a crystalline transition metal oxide from a transition metal ore. The method comprises providing the transition metal ore and then converting the transition metal ore to a crystalline transition metal oxide via microwave or laser irradiation. The microwave or laser irradiation are used to form the crystalline transition metal oxide as an alternative to using TMDs, which suffer from issues described herein. The crystalline transition metals oxides, (TMOs) have been found to be more potent than TMDs in energy generation and energy storage applications.

As described herein, rather than roasting the sulfide ores as has previously been the method in the art, the inventors have developed a method for converting transition metal ores to their oxide via microwave or laser irradiation. Generally, a microwave oven of power 800 W can be used, which is effective in producing crystalline TMOs. Similarly, a blue light (wavelength 450 nm) laser of power less than 100 W may be used to crystallize TMOs out of their ores (e.g., sulfides). Other microwave powers or laser powers may also be used to crystallize TMOs from their ores. This and other aspects of the invention are provided further below.

Transition metals ores refer to naturally occurring rocks or minerals found on earth. The ores contain a transition metal. Transition metals include scandium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, yttrium, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, lanthanum, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, mercury, actinium, rutherfordium, dubnium, seaborgium, bohrium, hassium, meitnerium, darmstadtium, roentgenium, and copernicium. The transition metal ore may comprise any or combinations of these transition metals.

In some aspects, the transition metal ore comprises from 1 to 95% of the transition metal, by weight, e.g., from 1 to 90%, from 1 to 85%, from 1 to 80%, from 1 to 75%, from 1 to 70%, from 1 to 65%, from 1 to 60%, from 1 to 55%, from 1 to 50%, from 1 to 45%, from 1 to 40%, from 1 to 35%, from 1 to 30%, from 1 to 25%, from 1 to 20%, from 1 to 15%, from 1 to 10%, from 1 to 5%, from 5 to 95%, from 5 to 90%, from 5 to 85%, from 5 to 80%, from 5 to 75%, from 5 to 70%, from 5 to 65%, from 5 to 60%, from 5 to 55%, from 5 to 50%, from 5 to 45%, from 5 to 40%, from 5 to 35%, from 5 to 30%, from 5 to 25%, from 5 to 20%, from 5 to 15%, from 5 to 10%, from 10 to 95%, from 10 to 90%, from 10 to 85%, from 10 to 80%, from 10 to 75%, from 10 to 70%, from 10 to 65%, from 10 to 60%, from 10 to 55%, from 10 to 50%, from 1 to 45%, from 10 to 40%, from 10 to 35%, from 10 to 30%, from 10 to 25%, from 10 to 20%, from 1 to 15%, from 15 to 95%, from 15 to 90%, from 15 to 85%, from 15 to 80%, from 15 to 75%, from 15 to 70%, from 15 to 65%, from 15 to 60%, from 15 to 55%, from 15 to 50%, from 15 to 45%, from 15 to 40%, from 15 to 35%, from 15 to 30%, from 15 to 25%, from 15 to 20%, from 20 to 95%, from 20 to 90%, from 20 to 85%, from 20 to 80%, from 20 to 75%, from 20 to 70%, from 20 to 65%, from 20 to 60%, from 20 to 55%, from 20 to 50%, from 20 to 45%, from 20 to 40%, from 20 to 35%, from 20 to 30%, from 20 to 25%, from 25 to 90%, from 25 to 85%, from 25 to 80%, from 25 to 75%, from 25 to 70%, from 25 to 65%, from 25 to 60%, from 25 to 55%, from 25 to 50%, from 25 to 45%, from 25 to 40%, from 25 to 35%, from 25 to 30%, from 30 to 95%, from 30 to 90%, from 30 to 85%, from 30 to 80%, from 30 to 75%, from 30 to 70%, from 30 to 65%, from 30 to 60%, from 30 to 55%, from 30 to 50%, from 30 to 45%, from 30 to 40%, from 30 to 35%, from 35 to 95%, from 35 to 90%, from 35 to 85%, from 35 to 80%, from 35 to 75%, from 35 to 70%, from 35 to 65%, from 35 to 60%, from 35 to 55%, from 35 to 50%, from 35 to 45%, from 35 to 40%, from 40 to 95%, from 40 to 90%, from 40 to 85%, from 40 to 80%, from 40 to 75%, from 40 to 70%, from 40 to 65%, from 40 to 60%, from 40 to 55%, from 40 to 50%, from 40 to 45%, from 45 to 95%, from 45 to 90%, from 45 to 85%, from 45 to 80%, from 45 to 75%, from 45 to 70%, from 45 to 65%, from 45 to 60%, from 45 to 55%, from 45 to 50%, from 50 to 95%, from 50 to 90%, from 50 to 85%, from 50 to 80%, from 50 to 75%, from 50 to 70%, from 50 to 65%, from 50 to 60%, from 50 to 55%, from 55 to 95%, from 55 to 90%, from 55 to 85%, from 55 to 80%, from 55 to 75%, from 55 to 70%, from 55 to 65%, from 55 to 60%, from 60 to 95%, from 60 to 90%, from 60 to 85%, from 60 to 80%, from 60 to 75%, from 60 to 70%, from 60 to 65%, from 65 to 90%, from 65 to 90%, from 65 to 85%, from 65 to 80%, from 65 to 75%, from 65 to 70%, from 70 to 95%, from 70 to 90%, from 70 to 85%, from 70 to 80%, from 70 to 75%, from 75 to 95%, from 75 to 90%, from 75 to 85%, from 75 to 80%, from 80 to 95%, from 80 to 90%, from 80 to 85%, from 85 to 95%, from 85 to 90%, or from 90to 95%.

In some aspects, the transition metal comprises chromite, pyrolusite, rhodochrosite, hematite, magnetite, laterite, pentlandite, chalcopyrite, malachite, sphalerite, zincite, zircon, columbite-tantalite, molybdenite, argentite, greenockite, or wolframite.

In some aspects, the transition metal ore has is a transition metal dichalcogenide (TMC). TMCs are a family of atomically thin, layered semiconducting materials having a formula of MX. M is a transition metal atom and X is a chalcogen atom. In some aspects, M may be Mn, Mo, Cr, Ti, V, Zr, Nb, Tc, Ta, Hf, W, or Re. X may be S, Se, or Te. The crystalline oxide formed corresponds to the oxide of the transition metal atom.

In some aspects, the transition metal ore comprises MoSe, MoS, WSe, WS, MoTe, or combinations thereof.

In some aspects, the transition metal ore comprises tungsten oxide, WO, or molybdenum sulfide, MoS.

In some aspects, the crystalline transition metal oxide is MoSand the is primarily alpha-MoS. In some aspects, the crystalline transition metal oxide is at least 55% alpha-MoS, at least 60% alpha-MoS, at least 65% alpha-MoS, at least 70% alpha-MoS, at least 75% alpha-MoS, at least 80% alpha-MoS, at least 85% alpha-MoS, at least 90% alpha-MoS, at least 55% alpha-MoS, or at least 99.9% alpha-MoS, In some aspects, the percentage of alpha-MoSmay range from 50 to 100% by weight, e.g., from 50 to 95% by weight, from 50 to 90% by weight, from 50 to 85% by weight, from 50 to 80% by weight, from 50 to 75% by weight, from 50 to 70% by weight, from 50 to 65% by weight, from 50 to 60% by weight, from 50 to 55% by weight, from 55 to 100% by weight, from 55 to 95% by weight, from 55 to 90% by weight, from 55 to 85% by weight, from 55 to 80% by weight, from 55 to 75% by weight, from 55 to 70% by weight, from 55 to 65% by weight, from 55 to 60% by weight, from 60 to 100% by weight, from 60 to 95% by weight, from 60 to 90% by weight, from 60 to 85% by weight, from 60 to 80% by weight, from 60 to 75% by weight, from 60 to 70% by weight, from 60 to 65% by weight, from 65 to 100% by weight, from 65 to 95% by weight, from 65 to 90% by weight, from 65 to 85% by weight, from 65 to 80% by weight, from 65 to 75% by weight, from 65 to 70% by weight, from 70 to 100% by weight, from 70 to 95% by weight, from 70 to 90% by weight, from 70 to 85% by weight, from 70 to 80% by weight, from 70 to 75% by weight, from 75 to 100% by weight, from 75 to 95% by weight, from 75 to 90% by weight, from 75 to 85% by weight, from 75 to 80% by weight, from 80 to 100% by weight, from 80 to 95% by weight, from 80 to 90% by weight, from 80 to 85% by weight, from 85 to 100% by weight, from 85 to 95% by weight, from 85 to 90% by weight, from 90 to 100% by weight, from 90 to 95% by weight, or from 95 to 100% by weight.

The method described herein may involve receiving a transition metal ore and generating a crystalline transition metal oxide corresponding to the transition metal ore. The ore may be converted to the corresponding oxide by applying a microwave power or a laser power to the transition metal orc.

In aspects where microwave power is applied, the microwave power may be provided at a power from 500 to 1200 W. In some aspects, the microwave power may be provided at from 500 to 1150 W, from 500 to 1100 W, from 500 to 1050 W, from 500 to 1000 W, from 500 to 950 W, from 500 to 900 W, from 500 to 850 W, from 500 to 800 W, from 500 to 750 W, from 500 to 700 W, from 500 to 650 W, from 500 to 600 W, from 500 to 550 W, from 550 to 1200 W, 550 to 1150 W, from 550 to 1100 W, from 550 to 1050 W, from 550 to 1000 W, from 550 to 950 W, from 550 to 900 W, from 550 to 850 W, from 550 to 800 W, from 550 to 750 W, from 550 to 700 W, from 550 to 650 W, from 550 to 600 W, from 600 to 1200 W, 600 to 1150 W, from 600 to 1100 W, from 600 to 1050 W, from 600 to 1000 W, from 600 to 950 W, from 600 to 900 W, from 600 to 850 W, from 600 to 800 W, from 600 to 750 W, from 600 to 700 W, from 600 to 650 W, from 650 to 1200 W, 650 to 1150 W, from 650 to 1100 W, from 650 to 1050 W, from 650 to 1000 W, from 650 to 950 W, from 650 to 900 W, from 650 to 850 W, from 650 to 800 W, from 650 to 750 W, from 650 to 700 W, from 700 to 1200 W, 700 to 1150 W, from 700 to 1100 W, from 700 to 1050 W, from 700 to 1000 W, from 700 to 950 W, from 700 to 900 W, from 700 to 850 W, from 700 to 800 W, from 700 to 750 W, from 750 to 1200 W, 750 to 1150 W, from 750 to 1100 W, from 750 to 1050 W, from 750 to 1000 W, from 750 to 950 W, from 750 to 900 W, from 750 to 850 W, from 750 to 800 W, from 800 to 1200 W, 800 to 1150 W, from 800 to 1100 W, from 800 to 1050 W, from 800 to 1000 W, from 800 to 950 W, from 800 to 900 W, from 800 to 850 W, from 850 to 1200 W, 850 to 1150 W, from 850 to 1100 W, from 850 to 1050 W, from 850 to 1000 W, from 850 to 950 W, from 850 to 900 W, from 900 to 1200 W, 900 to 1150 W, from 900 to 1100 W, from 900 to 1050 W, from 900 to 1000 W, from 900 to 950 W, from 950 to 1200 W, from 950 to 1150 W, from 950 to 1100 W, from 950 to 1050 W, from 950 to 1000 W, from 1000 to 1200 W, from 1000 to 1150 W, from 1000 to 1100 W, from 1000 to 1050 W, from 1050 to 1200 W, from 1050 to 1150 W, from 1050 to 1100 W, from 1100 to 1200 W, from 1100 to 1150 W, or from 1150 to 1200 W.

In some aspects, the microwave may be applied for 10 seconds to 5 minutes, e.g., from 10 seconds to 4 minutes, from 10 seconds to 3 minutes, from 10 seconds to 2 minutes, from 10 seconds to 1 minute, from 10 seconds to 30 seconds, from 30 seconds to 5 minutes, from 30 seconds to 4 minutes, from 30 seconds to 3 minutes, from 30 seconds to 2 minutes, from 30 seconds to 1 minute, from 1 minute to 5 minutes, from 1 minute to 4 minutes, from 1 minute to 3 minutes, from 1 minute to 2 minutes, from 2 minutes to 5 minutes, from 2 minutes to 4 minutes, from 2 minutes to 3 minutes, from 3 minutes to 5 minutes, from 3 minutes to 4 minutes, or from 4 minutes to 5 minutes. Following application of microwave irradiation, the graphene-infused wood is allowed to cool, such as at room temperature.

In some aspects, the crystalline transition metal oxide has crystals whether it is formed by microwave or laser. When the crystalline transition metal oxide is formed by microwave, it may comprise layered crystals. The layered crystals may have a larger size than the crystals formed by the laser process. In some aspects, the layered crystals formed by the microwave process may have a longest length from 0.1 to 5 microns, e.g., from 0.1 to 4 microns, from 0.1 to 3 microns, from 0.1 to 2 microns, from 0.2 to 1 micron, from 0.2 to 5 microns, from 0.2 to 4 microns, from 0.2 to 3 microns, from 0.2 to 2 microns, from 0.2 to 1 micron, from 0.3 to 5 microns, from 0.3 to 4 microns, from 0.3 to 3 microns, from 0.3 to 2 microns, from 0.3 to 1 micron, from 0.4 to 5 microns, from 0.4 to 4 microns, from 0.4 to 3 microns, from 0.4 to 2 micron, from 0.4 to 1 micron, from 0.5 to 5 microns, from 0.5 to 4 microns, from 0.5 to 3 microns, from 0.5 to 2 microns, from 0.5 to 1 micron, from 0.6 to 5 microns, from 0.6 to 4 microns, from 0.6 to 3 microns, from 0.6 to 2 microns, from 0.6 to 1 micron, from 0.7 to 5 microns, from 0.7 to 4 microns, from 0.7 to 3 microns, from 0.7 to 2 microns, from 0.7 to 1 micron, from 0.8 to 5 microns, from 0.8 to 4 microns, from 0.8 to 3 microns, from 0.8 to 2 microns, from 0.8 to 1 micron, from 0.9 to 5 microns, from 0.9 to 4 microns, from 0.9 to 3 microns, from 0.9 to 2 microns, from 0.9 to 1 micron, from 1 to 5 microns, from 1 to 4 microns, from 1 to 3 microns, from 1 to 2 microns, from 2 to 5 microns, from 2 to 4 microns, from 2 to 3 microns, from 3 to 5 microns, from 3 to 4 microns, or from 4 to 5 microns.

In some aspects, the crystalline transition metal oxide, when formed by laser, has microbelt crystals. The size of the microbelt may range, in a longest length from 10 to 1000 microns, e.g., from 10 to 950 microns, from 10 to 900 microns, from 10 to 850 microns, from 10 to 800 microns, from 10 to 750 microns, from 10 to 700 microns, from 10 to 650 microns, from 10 to 600 microns, from 10 to 550 microns, from 10 to 500 microns, from 10 to 450 microns, from 10 to 400 microns, from 10 to 350 microns, from 10 to 300 microns, from 10 to 250 microns, from 10 to 200 microns, from 10 to 150 microns, from 10 to 100 microns, from 10 to 50 microns, from 50 to 1000 microns, from 50 to 950 microns, from 50 to 900 microns, from 50 to 850 microns, from 50 to 800 microns, from 50 to 750 microns, from 50 to 700 microns, from 50 to 650 microns, from 50 to 600 microns, from 50 to 550 microns, from 50 to 500 microns, from 50 to 450 microns, from 50 to 400 microns, from 50 to 350 microns, from 50 to 300 microns, from 50 to 250 microns, from 50 to 200 microns, from 50 to 150 microns, from 50 to 100 microns, from 100 to 950 microns, from 100 to 900 microns, from 100 to 850 microns, from 100 to 800 microns, from 100 to 750 microns, from 100 to 700 microns, from 100 to 650 microns, from 100 to 600 microns, from 100 to 550 microns, from 100 to 500 microns, from 100 to 450 microns, from 100 to 400 microns, from 100 to 350 microns, from 100 to 300 microns, from 100 to 250 microns, from 100 to 200 microns, from 100 to 150 microns, from 150 to 950 microns, from 150 to 900 microns, from 150 to 850 microns, from 150 to 800 microns, from 150 to 750 microns, from 150 to 700 microns, from 150 to 650 microns, from 150 to 600 microns, from 150 to 550 microns, from 150 to 500 microns, from 150 to 450 microns, from 150 to 400 microns, from 150 to 350 microns, from 150 to 300 microns, from 150 to 250 microns, from 150 to 200 microns, from 200 to 950 microns, from 200 to 900 microns, from 200 to 850 microns, from 200 to 800 microns, from 200 to 750 microns, from 200 to 700 microns, from 200 to 650 microns, from 200 to 600 microns, from 200 to 550 microns, from 200 to 500 microns, from 200 to 450 microns, from 200 to 400 microns, from 200 to 350 microns, from 200 to 300 microns, from 200 to 250 microns, from 250 to 950 microns, from 250 to 900 microns, from 250 to 850 microns, from 250 to 800 microns, from 250 to 750 microns, from 250 to 700 microns, from 250 to 650 microns, from 250 to 600 microns, from 250 to 550 microns, from 250 to 500 microns, from 250 to 450 microns, from 250 to 400 microns, from 250 to 350 microns, from 250 to 300 microns, from 300 to 950 microns, from 300 to 900 microns, from 300 to 850 microns, from 300 to 800 microns, from 300 to 750 microns, from 300 to 700 microns, from 300 to 650 microns, from 300 to 600 microns, from 300 to 550 microns, from 300 to 500 microns, from 300 to 450 microns, from 300 to 400 microns, from 300 to 350 microns, from 350 to 950 microns, from 350 to 900 microns, from 350 to 850 microns, from 350 to 800 microns, from 350 to 750 microns, from 350 to 700 microns, from 350 to 650 microns, from 350 to 600 microns, from 350 to 550 microns, from 350 to 500 microns, from 350 to 450 microns, from 350 to 400 microns, from 400 to 950 microns, from 400 to 900 microns, from 400 to 850 microns, from 400 to 800 microns, from 400 to 750 microns, from 400 to 700 microns, from 400 to 650 microns, from 400 to 600 microns, from 400 to 550 microns, from 400 to 500 microns, from 400 to 450 microns, from 450 to 950 microns, from 450 to 900 microns, from 450 to 850 microns, from 450 to 800 microns, from 450 to 750 microns, from 450 to 700 microns, from 450 to 650 microns, from 450 to 600 microns, from 450 to 550 microns, from 450 to 500 microns, from 500 to 950 microns, from 500 to 900 microns, from 500 to 850 microns, from 500 to 800 microns, from 500 to 750 microns, from 500 to 700 microns, from 500 to 650 microns, from 500 to 600 microns, from 500 to 550 microns, from 550 to 950 microns, from 550 to 900 microns, from 550 to 850 microns, from 550 to 800 microns, from 550 to 750 microns, from 550 to 700 microns, from 550 to 650 microns, from 550 to 600 microns, from 600 to 950 microns, from 60 to 900 microns, from 600 to 850 microns, from 600 to 800 microns, from 600 to 750 microns, from 600 to 700 microns, from 600 to 650 microns, from 650 to 950 microns, from 650 to 900 microns, from 650 to 850 microns, from 650 to 800 microns, from 650 to 750 microns, from 650 to 700 microns, from 700 to 950 microns, from 700 to 900 microns, from 700 to 850 microns, from 700 to 800 microns, from 700 to 750 microns, from 750 to 1000 microns, from 750 to 950 microns, from 750 to 900 microns, from 750 to 850 microns, from 750 to 800 microns, from 800 to 1000 microns, from 800 to 950 microns, from 80 to 900 microns, from 850 to 1000 microns, from 850 to 950 microns, from 900 to 1000 microns, from 900 to 950 microns, or from 950 to 100 microns.

In some aspects, when a laser is applied, it may be applied at a power from 1 to 100 W. In some aspects, the laser may be applied at a power from 5 to 100 W, from 5 to 95 W, from 5 to 90 W, from 5 to 85 W, from 5 to 80 W, from 5 to 75 W, from 5 to 70 W, from 5 to 65 W, from 5 to 60 W, from 5 to 55 W, from 5 to 50 W, from 5 to 45 W, from 5 to 40 W, from 5 to 35 W, from 5 to 30 W, from 5 to 25 W, from 5 to 20 W, from 5 to 15 W, from 5 to 10 W, from 10 to 100 W, from 10 to 95 W, from 10 to 90 W, from 10 to 85 W, from 10 to 80 W, from 10 to 75 W, from 10 to 70 W, from 10 to 65 W, from 10 to 60 W, from 10 to 55 W, from 10 to 50 W, from 10 to 45 W, from 10 to 40 W, from 10 to 35 W, from 10 to 30 W, from 10 to 25 W, from 10 to 20 W, from 10 to 15 W, from 15 to 100 W, from 15 to 95 W, from 15 to 90 W, from 15 to 85 W, from 15 to 80 W, from 15 to 75 W, from 15 to 70 W, from 15 to 65 W, from 15 to 60 W, from 15 to 55 W, from 15 to 50 W, from 5 to 45 W, from 15 to 40 W, from 15 to 35 W, from 15 to 30 W, from 15 to 25 W, from 15 to 20 W, from 20 to 100 W, from 20 to 95 W, from 20 to 90 W, from 20 to 85% W from 20 to 80 W, from 20 to 75 W, from 20 to 70 W, from 20 to 65 W, from 20 to 60 W, from 20 to 55 W, from 20 to 50 W, from 20 to 45 W, from 20 to 40 W, from 20 to 35 W, from 20 to 30 W, from 20 to 25 W, from 25 to 100 W, from 25 to 95 W, from 25 to 90 W, from 25 to 85 W, from 5 to 80 W, from 25 to 75 W, from 25 to 70 W, from 25 to 65 W, from 25 to 60 W, from 25 to 55 W, from 25 to 50 W, from 25 to 45 W, from 25 to 40 W, from 25 to 35 W, from 25 to 30 W, from 30 to 100 W, from 30 to 95 W, from 30 to 90 W, from 30 to 85 W, from 30 to 80 W, from 30 to 75 W, from 30 to 70 W, from 30 to 65 W, from 30 to 60 W, from 30 to 55 W, from 30 to 50 W, from 30 to 45 W, from 30 to 40 W, from 30 to 35 W, from 35 to 100 W, from 35 to 95 W, from 35 to 90 W, from 35 to 85 W, from 35 to 80 W, from 35 to 75 W, from 35 to 70 W, from 35 to 65 W, from 35 to 60 W, from 35 to 55 W, from 35 to 50 W, from 35 to 45 W, from 35 to 40 W, from 40 to 100 W, from 40 to 95 W, from 40 to 90 W, from 40 to 85 W, from 40 to 80 W, from 40 to 75 W, from 40 to 70 W, from 40 to 65 W, from 40 to 60 W, from 40 to 55 W, from 40 to 50 W, from 40 to 45 W, from 45 to 100 W, from 45 to 95 W, from 45 to 90 W, from 45 to 85 W, from 45 to 80 W, from 45 to 75 W, from 45 to 70 W, from 45 to 65 W, from 45 to 60 W, from 45 to 55 W, from 45 to 50 W, from 50 to 100 W, from 50 to 95 W, from 50 to 90 W, from 50 to 85 W, from 50 to 80 W, from 50 to 75 W, from 50 to 70 W, from 50 to 65 W, from 50 to 60 W, from 50 to 55 W, from 55 to 100 W, from 55 to 95 W, from 55 to 90 W, from 55 to 85 W, from 55 to 80 W, from 55 to 75 W, from 55 to 70 W, from 55 to 65 W, from 55 to 60 W, from 60 to 100 W, from 60 to 95 W, from 60 to 90 W, from 60 to 85 W, from 60 to 80 W, from 60 to 75 W, from 60 to 70 W, from 60 to 65 W, from 65 to 100 W, from 65 to 95 W, from 65 to 90 W, from 65 to 85 W, from 65 to 80 W, from 65 to 75 W, from 65 to 70 W, from 70 to 100 W, from 70 to 95 W, from 70 to 90 W, from 70 to 85 W, from 70 to 80 W, from 70 to 75 W, from 75 to 100 W, from 75 to 95 W, from 75 to 90 W, from 75 to 85 W, from 75 to 80 W, from 80 to 100 W, from 80 to 95 W, from 80 to 90 W, from 80 to 85 W, from 85 to 100 W, from 85 to 95 W, from 85 to 90 W, from 90 to 100 W, from 90 to 95 W, from 95 to 100 W.

The laser may be a blue light having a wavelength from 380 to 500 nm. In some aspects, the wavelength of the laser is from 380 to 490 nm, from 380 to 480 nm, from 380 to 470 nm, from 380 to 460 nm, from 380 to 450 nm, from 380 to 440 nm, from 380 to 430 nm, from 380 to 420 nm, from 380 to 410 nm, from 380 to 400 nm, from 380 to 390 nm, from 390 to 500 nm, from 390 to 490 nm, from 390 to 480 nm, from 390 to 470 nm, from 390 to 460 nm, from 390 to 450 nm, from 390 to 440 nm, from 390 to 430 nm, from 390 to 420 nm, from 390 to 410 nm, from 390 to 400 nm, from 400 to 500 nm, 400 to 490 nm, from 400 to 480 nm, from 400 to 470 nm, from 400 to 460 nm, from 400 to 450 nm, from 400 to 440 nm, from 400 to 430 nm, from 400 to 420 nm, from 400 to 410 nm, from 410 to 500 nm, from 410 to 490 nm, from 410 to 480 nm, from 410 to 470 nm, from 410 to 460 nm, from 410 to 450 nm, from 410 to 440 nm, from 410 to 430 nm, from 410 to 420 nm, from 420 to 500 nm, from 420 to 490 nm, from 420 to 480 nm, from 420 to 470 nm, from 420 to 460 nm, from 420 to 450 nm, from 420 to 440 nm, from 420 to 430 nm, from 430 to 500 nm, from 430 to 490 nm, from 430 to 480 nm, from 430 to 470 nm, from 430 to 460 nm, from 430 to 450 nm, from 430 to 440 nm, from 440 to 500 nm, from 440 to 490 nm, from 440 to 480 nm, from 440 to 470 nm, from 440 to 460 nm, from 440 to 450 nm, from 450 to 500 nm, from 450 to 490 nm, from 450 to 480 nm, from 450 to 470 nm, from 450 to 460 nm, from 460 to 500 nm, from 460 to 490 nm, from 460 to 480 nm, from 460 to 470 nm, from 470 to 500 nm, from 470 to 490 nm, from 470 to 480 nm, from 480 to 500 nm, from 480 to 490 nm, or from 490 to 500 nm.

In some aspects, the laser may be applied for 5 seconds to 1 minute, such as from 5 seconds to 50 seconds, from 5 seconds to 40 seconds, from 5 seconds to 30 seconds, from 5 seconds to 20 seconds, from 5 seconds to 10 seconds, from 10 seconds to 1 minute, from 10 seconds to 50 seconds, from 10 seconds to 40 seconds, from 10 seconds to 30 seconds, from 10 seconds to 20 seconds, from 20 seconds to 1 minute, from 20 seconds to 50 seconds, from 20 seconds to 40 seconds, from 20 seconds to 30 seconds, from 30 seconds to 1 minute, from 30 seconds to 50 seconds, from 30 seconds to 40 seconds, from 40 seconds to 1 minute, from 40 seconds to 50 seconds, or from 50 seconds to 1 minute. Following application of laser irradiation, the graphene-infused wood is allowed to cool, such as at room temperature.

In some aspects, the crystalline metal oxide comprises less than 5 ppm impurities after the method is completed. In some aspects, the crystalline metal oxide comprises less than 1 ppm impurities or comprises no detectable impurities, as measured by EDX (energy dispersive x-ray spectroscopy). Following the irradiation by microwave or laser, no further washing or purifying is required.

The present disclosure may be further understood in view of the below non-limiting examples.

Example 1: Commercially available MOS2 powder from Sigma Aldrich was used as the starting material. Crystalline MoO3 was prepared by applying (a) microwave at 800 W and (b) laser at wavelength 450 (blue light) with less than 100 W power. The observed scanning electron microscope (SEM) images inandA-Cshow MoOcrystals formed via both microwave () and laser irradiation (). The scale foris 1 micron, with each figure showing different images and levels. The scale forismicrons, the scale foris 20 microns, and the scale foris 50 microns. The features of the crystalline MoOwere different betweenand, depending on the method used. While the microwave process causes larger layered crystals to form, the laser-based process resulted in the formation of micro belts, which is also a characteristic of MoOcrystals found in the literature.

The MoOformed by each method was then tested using Energy dispersive X-ray spectroscopy (EDX) to confirm the formation of impurity free and crystalline TMOs.shows the SEM image then tested by EDX and reported in.shows the SEM image then tested by EDX and reported in. As shown, in both, only Mo and O peaks can be seen, which was indicative of the formation of MoOwithout any other impurities. Also, EDX showed some distinct features for both processes as the SEM images suggested.

In order to confirm the SEM and EDX data, X-ray diffraction (XRD) was also carried out to confirm the signatures and kinds of MoOformed in this process.and B show the XRD patterns of both microwave () and laser produced () MoO. From the XRD data, while it is clear that both processes result in the production of the most stable form of MoO(i.e., alpha-MoO), there are still distinct peaks from both processes suggesting a different product formed with respect to the process.

While the invention has been described in detail, modifications within the spirit and scope of the invention will be readily apparent to those of skill in the art. It should be understood that aspects of the invention and portions of various embodiments and various features recited above and/or in the appended claims may be combined or interchanged either in whole or in part. In the foregoing descriptions of the various embodiments, those embodiments which refer to another embodiment may be appropriately combined with other embodiments as will be appreciated by one of ordinary skill in the art. Furthermore, those of ordinary skill in the art will appreciate that the foregoing description is by way of example only, and is not intended to limit the invention.