# US 10,369,086 B2 · Composite material having ceramic fibers

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- Number: US 10,369,086 B2
- Document ID: US10369086B2
- Status: Granted
- Kind: B2
- Application number: 15/552,751
- Filed: 2016-03-01
- Published: 2018-02-01
- Granted: 2019-08-06
- Earliest claimed: 2015-03-05
- Assignees: 3M Innovative Properties Company
- Applicants: 3M Innovative Properties Company
- Inventors: Bradley D. Craig; Gregory A. Kobussen
- Web page: https://patentgrep.com/patent/US10369086B2

## CPC

- A61K 6/16: Refractive index
- A61K 6/17: Particle size
- A61K 6/20: Protective coatings for natural or artificial teeth, e.g. sealings, dye coatings or varnish
- A61K 6/71: Fillers
- A61K 6/802: comprising ceramics
- A61K 6/887: Compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- 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)

## Abstract

The present disclosure provides a composite material, a method of making and using the composite material and dental products made by hardening the composite material. The composite material includes a polymerizable component, ceramic fibers and nanoclusters. Each of the ceramic fibers of the composite material has a length and where the length of fifty percent of the ceramic fibers, based on a total number of the ceramic fibers, is at least 50 micrometers and the length of ninety percent of the ceramic fibers, based on the total number of the ceramic fibers, is no greater than 500 micrometers. The composite material can also include discrete non-fumed metal oxide nanoparticles. The composite material can be hardened to become any one of a dental restorative, a dental adhesive, a dental mill blank, a dental cement, a dental prostheses, an orthodontic device, an orthodontic adhesive, a dental casting material or a dental coating.

## Claims

### Claim 1

A composite material, comprising:
20 to 40 weight percent (wt. %) of a polymerizable component;
4 to 50 wt. % of ceramic fibers; and
20 to 70 wt. % of nanoclusters, where the wt. % values of the composite material are based on a total weight of the composite material and total to a value of 100 wt. %, and where each of the ceramic fibers has a length and where the length of fifty percent of the ceramic fibers, based on a total number of the ceramic fibers, is at least 50 micrometers and the length of ninety percent of the ceramic fibers, based on the total number of the ceramic fibers, is no greater than 500 micrometers.

### Claim 2 (depends on 1)

The composite material of claim 1, where the composite material includes up to 12 wt. % of nanoparticles.

### Claim 3 (depends on 2)

The composite material of claim 2, where the composite material includes 2 to 12 wt. % of nanoparticles.

### Claim 4 (depends on 3)

The composite material of claim 3, where the nanoparticles are discrete non-fumed metal oxide nanoparticles.

### Claim 5 (depends on 4)

The composite material of claim 4, where the discrete non-fumed metal oxide nanoparticles are discrete non-fumed heavy metal oxide nanoparticles.

### Claim 6 (depends on 4)

The composite material of claim 4, where the discrete non-fumed metal oxide nanoparticles include both discrete non-fumed heavy metal oxide nanoparticles and discrete non-fumed non-heavy metal oxide nanoparticles.

### Claim 7 (depends on 1)

The composite material of claim 1, where the composite material includes 22 to 64 wt. % of nanoclusters.

### Claim 8 (depends on 1)

The composite material of claim 1, where the ceramic fibers are at least partially amorphous ceramic fibers.

### Claim 9 (depends on 8)

The composite material of claim 8, where the ceramic fibers are completely amorphous ceramic fibers.

### Claim 10 (depends on 1)

The composite material of claim 1, where the composite material includes 4 to 40 wt. % of the ceramic fibers based on the total weight of the composite material.

### Claim 11 (depends on 1)

The composite material of claim 1, where the length of sixty-five percent of the ceramic fibers, based on a total number of the ceramic fibers, is at least 100 micrometers and the length of ninety percent of the ceramic fibers, based on the total number of the ceramic fibers, is no greater than 350 micrometers.

### Claim 12 (depends on 1)

The composite material of claim 1, where the ceramic fibers have an arithmetic mean length of 100 micrometers to 170 micrometers.

### Claim 13 (depends on 1)

The composite material of claim 1, where the ceramic fibers have an arithmetic mean diameter of 0.5 to 20 micrometers.

### Claim 14 (depends on 13)

The composite material of claim 13, where the arithmetic mean diameter of the ceramic fibers is 9 to 12 micrometers.

### Claim 15 (depends on 1)

The composite material of claim 1, where an aspect ratio of a median length of the fifty percent of the ceramic fibers that are at least 50 micrometers to a median diameter of the fifty percent of the ceramic fibers that are at least 50 micrometers is at least 5:1 (median length:median diameter).

### Claim 16 (depends on 1)

The composite material of claim 1, where the ceramic fibers are formed with aluminum oxide and silicon dioxide and have 14 weight percent or less of boron trioxide based on the total weight of the ceramic fibers.

### Claim 17 (depends on 1)

The composite material of claim 1, where the ceramic fibers have a surface area of at least 10 square meters per gram (m2/g).

### Claim 18 (depends on 1)

The composite material of claim 1, where the polymerizable component forms a hardened polymerizable component having a refractive index, where the ceramic fibers have a refractive index value within 0.1 or less of the refractive index of the hardened polymerizable component.

### Claim 19 (depends on 18)

The composite material of claim 18, where the ceramic fibers have a refractive index value within 0.05 or less of the refractive index of the hardened polymerizable component.

### Claim 20 (depends on 1)

The composite material of claim 1, where the ceramic fibers have a refractive index value of 1.40 to 1.65.

### Claim 21 (depends on 20)

The composite material of claim 20, where the refractive index value of the ceramic fibers is 1.50 to 1.58.

### Claim 22 (depends on 1)

The composite material of claim 1, wherein the polymerizable component is an ethylenically unsaturated compound.

### Claim 23 (depends on 1)

The composite material of claim 1, further including an initiator selected from the group consisting of a free radical initiator, a photoinitiator, a thermally activated initiator or a combination thereof.

### Claim 24 (depends on 1)

The composite material of claim 1, further including a coupling agent, where the coupling agent provides a chemical bond between the ceramic fibers and the polymerizable component.

### Claim 25 (depends on 24)

The composite material of claim 24, where the coupling agent is selected from the group consisting of an organosilane coupling agent, a titanate coupling agent, a zirconate coupling agent, an acidic coupling agent or a combination thereof.

### Claim 26 (depends on 1)

The composite material of claim 1, where the composite material is hardened to become any one of a dental restorative, a dental adhesive, a dental mill blank, a dental cement, a dental prostheses, an orthodontic device, an orthodontic adhesive, a dental casting material or a dental coating.

### Claim 27 (depends on 1)

The composite material of claim 1, where the nanoclusters are silica-zirconia nanoclusters.

### Claim 28 (depends on 27)

The composite material of claim 27, where the silica-zirconia nanoclusters are formed by primary particles, where each of the primary particles has a diameter of 1 nanometer to 200 nanometers.
