# US 9,517,361 B2 · Crystal encapsulated nanoparticles methods and compositions

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- Number: US 9,517,361 B2
- Document ID: US9517361B2
- Status: Granted
- Kind: B2
- Application number: 13/652,051
- Filed: 2012-10-15
- Published: 2015-06-25
- Granted: 2016-12-13
- Earliest claimed: 2011-10-17
- Assignees: Purdue Research Foundation
- Applicants: David A. Reese; Steven F. Son; Allen Hoe Yan
- Inventors: David A. Reese; Steven F. Son; Allen Hoe Yan
- Web page: https://patentgrep.com/patent/US9517361B2

## CPC

- A61K 9/5192: {Processes}
- A61K 8/0241: {Containing particulates characterized by their shape and/or structure (see also A61K8/04, A61K8/11, and A61K8/14, further aspects are classified in A61K2800/40 and subcodes)}
- A61K 8/8194: {Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, at least one having two or more carbon-to-carbon double bonds; Compositions of derivatives of such polymers}
- A61K 9/16: Agglomerates; Granulates; Microbeadlets {; Microspheres; Pellets; Solid products obtained by spray drying, spray freeze drying, spray congealing,(multiple) emulsion solvent evaporation or extraction (A61K9/20 takes precedence if the final form is a tablet; microspheres with drug-free outer coating, microcapsules A61K9/50; mixture of different granules, microcapsules, (coated) microparticles A61K9/5084; nanoparticles A61K9/51)}
- A61K 9/5115: {Inorganic compounds}
- A61Q 1/02: Preparations containing skin colorants, e.g. pigments (preparations in powder form A61Q1/12)
- A61Q 19/00: Preparations for care of the skin
- C06B 45/02: comprising particles of diverse size or shape
- C06B 45/18: comprising a coated component (particles dispersed in a matrix C06B45/04; coated explosive charges F42B)
- C06B 45/32: the coating containing an organic compound
- A61K 2800/10: General cosmetic use
- A61K 2800/413: Nanosized, i.e. having sizes below 100 nm
- A61K 2800/624: by macromolecular compounds
- Y10T 428/2991: Coated
- A61K: PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES (devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms A61J3/00; chemical aspects of, or use of materials for deodorisation of air, for disinfection or sterilisation, or for bandages, dressings, absorbent pads or surgical articles A61L; soap compositions C11D)
- A61Q: SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- C06B: EXPLOSIVES OR THERMIC COMPOSITIONS (blasting F42D); MANUFACTURE THEREOF; USE OF SINGLE SUBSTANCES AS EXPLOSIVES (compounds in general C01, C07 or C08; {demolition agents based on cementitious or like materials C04B41/0009})
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

The invention provides methods for encapsulating nanometric particles inside of micro-sized crystals. An exemplary embodiment involves crystallizing a solution including nanometric particles, a micelle-forming material, a nonpolar dispersant for the micelle-forming material and a crystal-forming material to form crystal-encapsulated nanometric particles. Also provided are compositions or materials which include or are formed using the crystal encapsulated nanoparticles, such compositions and materials can include propellants, cosmetics, composite structures, energetics, and pharmaceutical compositions/materials.

## Claims

### Claim 1

A method for making a composite of nanometric particles encapsulated by crystals, said method comprising:
crystallizing a solution comprising nanometric particles, a micelle-forming material, a nonpolar dispersant for the micelle-forming material and a crystal-forming material to form crystal-encapsulated nanometric particles.

### Claim 2 (depends on 1)

The method of claim 1 wherein said nanometric particles comprise a nanometric particle selected from the group consisting of iron oxide (nanocat), nanoaluminum, nanoboron, boron-nitride nanotubes (BNNT), nanodiamond, and combinations of two or more thereof.

### Claim 3 (depends on 2)

The method of claim 2 wherein said nanometric particles comprise iron oxide.

### Claim 4 (depends on 1)

The method of claim 1 wherein said crystal-forming material comprises ammonium perchlorate.

### Claim 5 (depends on 1)

The method of claim 1 wherein said micelle-forming material is hydroxyl terminated polybutadiene.

### Claim 6 (depends on 1)

The method of claim 1 wherein said nonpolar dispersant comprises pentane.

### Claim 7 (depends on 1)

The method of claim 1 wherein said crystallizing is carried out by drying.

### Claim 8 (depends on 1)

The method of claim 1 wherein said micelle-forming material and said nonpolar dispersant are combined with a suitable solvent prior to said crystallizing.

### Claim 9 (depends on 8)

The method of claim 8 wherein said crystal-forming material is added to the combination of said micelle-forming material, said nonpolar dispersant and said solvent.

### Claim 10 (depends on 9)

The method of claim 9 wherein said crystal-forming material is a salt and said salt is substantially or completely dissolved in said solution.

### Claim 11 (depends on 10)

The method of claim 10 wherein said dissolving is carried out by mechanical agitation or temperature change.

### Claim 12 (depends on 10)

The method of claim 10 wherein said nanometric particles are added to said micelle-forming material, said nonpolar dispersant and said salt.

### Claim 13 (depends on 12)

The method of claim 12 wherein said nanometric particles are dispersed in said polar solvent, said micelle-forming material, said non-polar dispersant, and said salt.

### Claim 14 (depends on 13)

The method of claim 13 wherein said dispersion is carried out by mechanical agitation.

### Claim 15 (depends on 1)

The method of claim 1 wherein nanometric iron oxide particles are encapsulated inside of micrometric ammonium perchlorate crystals, the method comprising:
preparing a solution including nanometric iron oxide and ammonium perchlorate with a micelle-forming material and a polar dispersant for the micelle-forming material; and
said crystallizing step comprises crystallizing the solution to form nanometric iron oxide particles encapsulated inside of micrometric ammonium perchlorate crystals.

### Claim 16 (depends on 15)

The method of claim 15 wherein the micelle-forming material comprises hydroxyl terminated polybutadiene.

### Claim 17 (depends on 15)

The method of claim 15 wherein said crystallizing is carried out by drying.

### Claim 18

A method for making a core-shell composite material, said method comprising:
crystallizing a solution comprising nanometric particles, a micelle-forming material, a nonpolar dispersant for the micelle-forming material and a crystal-forming material to form the core-shell composite material wherein nanometric particles form a core within a micron-sized crystal shell.