Fracture-resistant layered-substrates and articles including the same

• US 10,160,688 B2
• Filed: 09/10/2014
• Issued: 12/25/2018
• Est. Priority Date: 09/13/2013
• Status: Active Grant

• Current Assignee: Corning Incorporated
• Original Assignee: Corning Incorporated
• Inventors: Amin, Jaymin, Mayolet, Alexandre Michel, Paulson, Charles Andrew, Price, James Joseph, Reiman, Kevin Barry
• Primary Examiner(s): Colgan, Lauren R
• Application Number:
  US14/482,250
• Publication Number:
  US 20150079398A1
• Time in Patent Office: 1,567 Days
• Field of Search: 428426, 428428, 428432, 428433, 428434, 428688, 428689, 428697, 428698, 428699, 428701, 428702, 428409, 428410
• CPC Class Codes: C01B 21/068 with silicon
• CPC Class Codes: C01B 21/072 with aluminium
• CPC Class Codes: C01B 21/0823 Silicon oxynitrides
• CPC Class Codes: C01B 21/0825 Aluminium oxynitrides
• CPC Class Codes: C03C 17/22 with other inorganic material C03C17/34, C03C17/44 take precedence
• CPC Class Codes: C03C 17/225 Nitrides
• CPC Class Codes: C03C 17/3435 comprising a nitride, oxynitride, boronitride or carbonitride
• CPC Class Codes: C03C 21/002 to perform ion-exchange between alkali ions C03C21/005 takes precedence
• CPC Class Codes: C03C 2217/28 Other inorganic materials
• CPC Class Codes: C03C 2217/281 Nitrides
• CPC Class Codes: C03C 2217/78 Coatings specially designed to be durable, e.g. scratch-resistant
• CPC Class Codes: C03C 2217/91 Coatings containing at least one layer having a composition gradient through its thickness
• CPC Class Codes: C03C 3/091 containing aluminium
• CPC Class Codes: G01N 2203/0098 Tests specified by its name, e.g. Charpy, Brinnel, Mullen
• CPC Class Codes: G01N 3/42 by performing impressions under a steady load by indentors, e.g. sphere, pyramid G01N3/54 takes precedence
• CPC Class Codes: H04M 1/185 Improving the rigidity of the casing or resistance to shocks
• CPC Class Codes: Y10T 428/30 Self-sustaining carbon mass or layer with impregnant or other layer

Abstract

Embodiments of a layered-substrate comprising a substrate and a layer disposed thereon, wherein the layered-substrate is able to withstand fracture when assembled with a device that is dropped from a height of at least 100 cm onto a drop surface, are disclosed. The layered-substrate may exhibit a hardness of at least about 10 GPa or at least about 20 GPa. The substrate may include an amorphous substrate or a crystalline substrate. Examples of amorphous substrates include glass, which is optionally chemically strengthened. Examples of crystalline substrates include single crystal substrates (e.g. sapphire) and glass ceramics. Articles and/or devices including such layered-substrate and methods for making such devices are also disclosed.

Claims

1. A layered-substrate comprising:

a substrate comprising an outwardly-facing surface;

a layer disposed on the outwardly-facing surface, wherein the layered-substrate exhibits a hardness of at least about 12 GPa, as measured by the Berkovich Indenter Hardness Test, along an indentation depth of about 100 nm or greater and wherein the layered-substrate is able to withstand fracture when assembled in a device and the device is dropped from a height of at least 100 cm onto a drop surface, wherein the layer comprises 55 or more % by weight of a metal oxynitride, and;

an additional layer comprising metal oxide, wherein the additional layer is disposed directly on the layer so that the layer is disposed between the substrate and the additional layer.

2. The layered-substrate of claim 1, wherein the outwardly facing surface comprises at least one of opposing major surfaces, and the substrate exhibits an average strain-to-failure at a surface of one or more of the opposing major surfaces that is 0.5% or greater.

3. The layered-substrate of claim 1, wherein the substrate is chemically strengthened and comprises a compressive stress (CS) layer with a CS of at least 250 MPa extending to a depth of layer (DOL) of at least 10 μ

m.

4. The layered-substrate of claim 1, wherein the layer exhibits a hardness of at least about 20 GPa, as measured by a Berkovich Indenter Hardness Test, along an indentation depth of about 100 nm or greater, and has a thickness of at least about 500 nm.

5. The layered-substrate of claim 1, wherein the layered-substrate exhibits a transmittance of at least about 85%, or of less than about 10%, over the visible spectrum.

6. The layered-substrate of claim 1, wherein the layer has a first index of refraction, the additional layer has a second index of refraction, and further wherein the first index of refraction is higher than the second index of refraction.

7. The layered-substrate of claim 1, further comprising a second additional layer comprising metal oxide, wherein the second additional layer is disposed directly on the substrate so that the second additional layer is disposed between the layer and the substrate.

8. The layered-substrate of claim 7, wherein the metal oxynitride comprises silicon oxynitride, and the metal oxide comprises silicon oxide.

9. A fracture-resistant article comprising:

a substrate comprising opposing major surfaces;

a layer disposed on a first opposing major surface of the substrate, wherein the article exhibits a hardness of at least about 10 GPa as measured by a Berkovich Indenter Hardness Test along an indentation depth of about 100 nm or greater, and is able to withstand fracture when assembled with a device that is dropped in a drop test from a height of at least 100 cm onto a drop surface, wherein the layer comprises 55 or more % by weight of a metal oxynitride, and;

an additional layer comprising metal oxide, wherein the additional layer is disposed directly on the layer so that the layer is disposed between the substrate and the additional layer.

10. The fracture-resistant article of claim 9, wherein the drop surface comprises asphalt or 180 grit sandpaper.

11. The fracture-resistant article of claim 9, wherein the substrate exhibits an average strain-to-failure at a surface of one or more of the opposing major surfaces that is 0.5% or greater.

12. The fracture-resistant article of claim 9, wherein the substrate is chemically strengthened and comprises a compressive stress (CS) layer with a CS of at least 250 MPa extending to a depth of layer (DOL) of at least 10 μ

m.

13. The fracture-resistant article of claim 9, wherein the metal of the metal oxynitride is selected from the group consisting of B, Al Si, Ti, V, Cr, Y, Zr, Nb, Mo, Sn, Hf, Ta and W.

14. The fracture-resistant article of claim 9, further exhibiting resistance to flaw penetration of one or more flaws from the layer, wherein the one or more flaws from the layer comprise at least one of:

flaws that are introduced into the layer by contact between the layered-substrate and the drop surface; and

flaws that are present in the layer prior to being dropped.

15. The fracture-resistant article of claim 14, wherein the layer substantially prevents the introduction of new flaws into the substrate.

16. The layered-substrate of claim 9, wherein the layer has a first index of refraction, the additional layer has a second index of refraction, and further wherein the first index of refraction is higher than the second index of refraction.

17. The layered-substrate of claim 9, further comprising a second additional layer comprising metal oxide, wherein the second additional layer is disposed directly on the substrate so that the second additional layer is disposed between the layer and the substrate.

18. The layered-substrate of claim 17, wherein the metal oxynitride comprises silicon oxynitride, and the metal oxide comprises silicon oxide.

19. A portable device comprising:

a substrate having a major surface providing a user interface and having an initial scratch resistance and an initial impact resistance;

a layer on the major surface forming a layered-substrate exhibiting an enhanced scratch resistance and enhanced impact resistance, wherein the enhanced impact resistance comprises an average flexural strength after abrading the layered-substrate that is at least 80% of an average flexural strength before abrading the layered-substrate, and wherein said enhanced scratch resistance comprises a hardness of at least about 10 GPa, as measured by a Berkovich Indenter Hardness Test, along an indentation depth of about 100 nm or greater, wherein the layer comprises 55 or more % by weight of a metal oxynitride, and;

an additional layer comprising metal oxide, wherein the additional layer is disposed directly on the layer so that the layer is disposed between the substrate and the additional layer.

20. A device comprising:

a substrate comprising opposing major surfaces;

a layer disposed on a first opposing major surface of the substrate to form a layered-substrate, wherein the layered-substrate is able to withstand fracture when the device is dropped from a height of at least 100 cm onto a drop surface, wherein the layer comprises 55 or more by weight of a metal oxynitride, and;

an additional layer comprising metal oxide, wherein the additional layer is disposed directly on the layer so that the layer is disposed between the substrate and the additional layer.