# US 10,370,305 B1 · Encapsulated polymer nanocomposite for efficient crack repair and monitoring of cement, rock, and other brittle materials

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- Number: US 10,370,305 B1
- Document ID: US10370305B1
- Status: Granted
- Kind: B1
- Application number: 15/681,981
- Filed: 2017-08-21
- Granted: 2019-08-06
- Earliest claimed: 2016-08-19
- Assignees: Stc.Unm
- Applicants: Stc.Unm
- Inventors: Mahmoud Reda Taha; John Stormont; Edward N. Matteo
- Web page: https://patentgrep.com/patent/US10370305B1

## CPC

- C04B 41/455: {the coating or impregnating process including a chemical conversion or reaction}
- C04B 40/0633: {Chemical separation of ingredients, e.g. slowly soluble activator}
- C04B 41/009: {characterised by the material treated}
- C04B 41/4535: {applied as a solution, emulsion, dispersion or suspension}
- C04B 41/457: {Non-superficial impregnation or infiltration of the substrate}
- C04B 41/483: {Polyacrylates}
- C04B 41/4853: {Epoxides}
- C04B 41/4884: {Polyurethanes; Polyisocyanates}
- C04B 41/4961: {Polyorganosiloxanes, i.e. polymers with a Si-O-Si-O-chain; "silicones"}
- C04B 41/5001: {with carbon or carbonisable materials}
- C04B 41/5006: {Boron compounds}
- C04B 41/53: involving the removal of at least part of the materials of the treated article, {e.g. etching, drying of hardened concrete (C04B41/0036 - C04B41/0054 take precedence)}
- C04B 41/72: involving the removal of part of the materials of the treated articles, e.g. etching
- C09D 7/70: {characterised by shape, e.g. fibres, flakes or microspheres}
- C09K 8/428: {for squeeze cementing, e.g. for repairing}
- C09K 8/44: containing organic binders only
- E21B 33/138: Plastering the borehole wall; Injecting into the formation
- E21B 43/267: reinforcing fractures by propping
- C04B 2111/00008: {Obtaining or using nanotechnology related materials}
- C04B 2111/00663: {as filling material for cavities or the like}
- C04B 2111/343: {Crack resistant materials}
- C04B 2111/346: {Materials exhibiting reduced plastic shrinkage cracking}
- C04B 2111/72: Repairing or restoring existing buildings or building materials
- C08K 9/10: Encapsulated ingredients
- C04B: LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE {(roofing granules E04D7/005)}; CERAMICS (devitrified glass-ceramics C03C10/00); REFRACTORIES; TREATMENT OF NATURAL STONE
- C09D: COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR (cosmetics A61K; processes for applying liquids or other fluent materials to surfaces, in general, B05D; staining wood B27K5/02; glazes or vitreous enamels C03C; natural resins, French polish, drying-oils, driers, turpentine, per se, C09F; polishing compositions other than French polish, ski waxes C09G; adhesives or use of materials as adhesives C09J; materials for sealing or packing joints or covers C09K3/10; materials for stopping leaks C09K3/12; processes for the electrolytic or electrophoretic production of coatings C25D)
- C09K: MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- E21B: EARTH OR ROCK DRILLING; OBTAINING OIL, GAS, WATER, SOLUBLE OR MELTABLE MATERIALS OR A SLURRY OF MINERALS FROM WELLS
- C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09)

## Abstract

The present invention concerns compositions and methods of using the same that provide encapsulated polymer nanocomposites for efficient crack repair and monitoring of a cement-substrate interface.

## Claims

### Claim 1

A microencapsulated crack arrest material comprising: a polymer matrix incorporating one or more microcapsules, said microcapsules rupture in response to a predetermined humidity gradient include materials that initiate cross-linking when contacting a catalyst.

### Claim 2 (depends on 1)

The material of claim 1 wherein said microcapsules rupture in response to a predetermined humidity gradient and a predetermined temperature gradient.

### Claim 3 (depends on 1)

The material of claim 1 wherein said microcapsules include dicyclopentadiene to initiate polymer cross-linking when contacting a catalyst.

### Claim 4 (depends on 1)

The material of claim 1 wherein said microcapsules rupture to release their contents to react with a catalyst in response a predetermined temperature gradient at one or more crack tips and bonds to the crack tip surface to prevent crack propagation.

### Claim 5 (depends on 1)

The material of claim 1 wherein said microcapsules include one or more materials from the group comprising: graphene nanoparticles, Novolac-epoxy, Novolac-epoxy incorporating carbon nanotubes, siloxane-epoxy incorporating MWCNTs; BNTs; MWCNTs or nanoalumina, methyl methacrylate, methyl methacrylate incorporating nanoalumina, methyl methacrylate incorporating MWCNTs.

### Claim 6 (depends on 5)

The material of claim 5 wherein said carbon nanotubes are adapted to disperse homogeneously in the matrix.

### Claim 7 (depends on 5)

The material of claim 5 wherein said carbon nanotubes are chemically modified to have an affinity toward solvent molecules, polymer matrices or generic reactants.

### Claim 8 (depends on 1)

The material of claim 1 wherein said microcapsules incorporate magnetic nanoparticles.

### Claim 9 (depends on 1)

The material of claim 1 further including one or more catalysts such as bis(tricyclohexylphosphine) benzylidine ruthenium (IV) dichloride.

### Claim 10 (depends on 1)

The material of claim 1 further including nanomaterials that enable ultrasonic monitoring of crack propagation and crack arrest.

### Claim 11

A microencapsulated crack arrest material comprising: a polymer matrix incorporating one or more microcapsules, said microcapsules incorporate magnetic nanoparticles and rupture in response to a predetermined humidity.

### Claim 12 (depends on 11)

The material of claim 11 wherein said microcapsules rupture in response to a predetermined humidity gradient and a predetermined temperature gradient.

### Claim 13 (depends on 11)

The material of claim 11 wherein said microcapsules include materials that initiate polymer cross-linking when contacting a catalyst.

### Claim 14 (depends on 13)

The material of claim 13 wherein said microcapsules include dicyclopentadiene to initiate polymer cross-linking when contacting a catalyst.

### Claim 15 (depends on 11)

The material of claim 11 wherein said microcapsules rupture to release their contents to react with a catalyst in response a predetermined temperature gradient at one or more crack tips and bonds to the crack tip surface to prevent crack propagation.

### Claim 16 (depends on 11)

The material of claim 11 wherein said microcapsules include one or more materials from the group comprising: graphene nanoparticles, Novolac-epoxy, Novolac-epoxy incorporating carbon nanotubes, siloxane-epoxy incorporating MWCNTs; BNTs; MWCNTs or nanoalumina, methyl methacrylate, methyl methacrylate incorporating nanoalumina, methyl methacrylate incorporating MWCNTs.

### Claim 17 (depends on 16)

The material of claim 16 wherein said carbon nanotubes are adapted to disperse homogeneously in the matrix.

### Claim 18 (depends on 16)

The material of claim 16 wherein said carbon nanotubes are chemically modified to have an affinity toward solvent molecules, polymer matrices or generic reactants.

### Claim 19 (depends on 11)

The material of claim 11 further including one or more catalysts such as bis(tricyclohexylphosphine) benzylidine ruthenium (IV) dichloride.

### Claim 20 (depends on 11)

The material of claim 11 further including nanomaterials that enable ultrasonic monitoring of crack propagation and crack arrest.