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Glass-ceramic articles with improved stress profiles

A technology of glass ceramics and stress distribution, applied in the field of glass ceramic products with improved stress distribution, which can solve the problems of slow diffusion

Active Publication Date: 2021-03-30
CORNING INC
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In general, K, being a larger ionic radius, induces higher stress, but diffuses slowly compared to smaller ionic radius Na ions, which induce lower stress
For this reason, it can be challenging to induce high stress at moderate depths when using mixed K / Na salt baths

Method used

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  • Glass-ceramic articles with improved stress profiles
  • Glass-ceramic articles with improved stress profiles
  • Glass-ceramic articles with improved stress profiles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0146] Glass-ceramic articles were formed from the above-mentioned lithium-based glass-ceramic substrates by a two-step ion exchange treatment.

[0147] The first IOX bath is 100 wt% KNO 3 , and 0.5% by weight (of the bath) of NaNO was added to the bath 2 Dose to improve bath chemistry. 10X at 460°C for 8 hours. After the first IOX with: 0.1824% weight gain, 435 MPa compressive stress (CS), depth of layer (DOL) for K 8.1 microns (depth of inflection point), 25.60 MPa maximum central tension (CT). figure 2 are images of TM and TE guided mode spectral fringes after the first 10X treatment.

[0148] The substrate is then exposed to a second 10× bath, which is 90% by weight KNO 3 and 10 wt% NaNO 3 , and contains (of the bath) 0.5% by weight of NaNO 2 dose. The second 10X was at 430°C for 8 hours. Has: 0.3463% weight gain, 339 MPa CS, DOL for K 9.4 microns, 39.75 MPa maximum central tension (CT). image 3 are images of the TM and TE guided mode spectral fringes of the res...

Embodiment 2

[0150] Glass-ceramic articles were formed from the above-mentioned lithium-based glass-ceramic substrates by a two-step ion exchange process in the presence of lithium in the IOX process.

[0151] The first IOX bath is 100 wt% KNO 3 , to which 0.02% by weight (of the bath) of LiNO was added 3 Dose and 0.5 wt% NaNO 2 dose. The first 10X was at 460°C for 8 hours. Has a 0.1219% weight gain and a CT of 17.36 MPa. Figure 4 are images of TM and TE guided mode spectral fringes after the first 10X treatment.

[0152] The substrate is then exposed to a second 10× bath, which is 90% by weight KNO 3 and 10 wt% NaNO 3 , to which 0.02 wt% (of the bath) of LiNO was added 3 Dose and 0.5 wt% NaNO 2 dose. The second 10X was at 430°C for 8 hours. Has a 0.3587% weight gain and a CT of 45.78 MPa. Figure 5 are images of the TM and TE guided mode spectral fringes of the resulting glass-ceramic article. There are two stripes, which enable proper process control over bath composition, b...

Embodiment 3

[0154] Glass-ceramic articles were formed from the above-mentioned lithium-based glass-ceramic substrates by a two-step ion exchange process in the presence of lithium in the IOX process.

[0155] The first IOX bath is 100 wt% KNO 3 , to which 0.02% by weight (of the bath) of LiNO was added 3 Dose and 0.5 wt% NaNO 2 dose. The first 10X was at 460°C for 8 hours. Has a CT of 15.97MPa. Figure 6 are images of TM and TE guided mode spectral fringes after the first 10X treatment. Figure 7 is the resulting stress profile (stress (MPa) vs. position (microns) plot) after the first 10× treatment for half the substrate thickness. exist Figure 7 , notice the presence of spikes.

[0156] The substrate is then exposed to a second 10× bath, which is 90% by weight KNO 3 and 10 wt% NaNO 3 , to which 0.02 wt% (of the bath) of LiNO was added 3 Dose and 0.5 wt% NaNO 2 dose. The second 10X was at 460°C for 10 hours. Has a CS of 303 MPa, a potassium DOL (depth of inflection point) o...

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Abstract

Glass-ceramic articles are manufactured by an ion exchange process that results in glass-based articles having improved stress profiles. A knee may be located at a depth of 3 microns or deeper. A compressive stress at a surface may be 200 MPa or more and at a knee may be 20 MPa or more. A non-sodium oxide may have a non-zero concentration that varies from the first surface to a depth and a depth of compression (DOC) may be located at 0.10t, or even at 0.17t or deeper. A two-step ion exchange (DIOX) includes, for example, a potassium bath in a first treatment to form a spike in a spike region of the stress profile, followed by a second treatment which includes, for example, a potassium and sodium mixed bath to maintain the spike and form a tail region of the stress profile. The glass-ceramic articles may thereby avoid developing a vitreous surface layer, which facilitates repeatable and reliable measurement of waveguide modes and determination of compressive stress in the surface (CS) and depth of the spike.

Description

[0001] Cross References to Related Applications [0002] This application claims priority under 35 U.S.C. §119 to U.S. Provisional Application Serial No. 62 / 719,730, filed August 20, 2018, which is hereby based and incorporated by reference in its entirety. technical field [0003] Embodiments of the present disclosure generally relate to glass-ceramic articles and high-strength glass-ceramic articles with improved stress distribution and methods of making the same. Background technique [0004] Glass-ceramic articles can be chemically strengthened, for example by ion exchange, to improve mechanical properties such as crack penetration and drop resistance. Glass ceramics are heterogeneous materials with one or more crystalline phases and residual glass phases, in which ion exchange processes can be complex. In addition to affecting the residual glass phase, ion exchange also affects one or more of the crystalline phases. [0005] Chemical treatment is a strengthening metho...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C03C21/00C03C10/00C03C3/097
CPCC03C21/002C03C10/0027C03C3/097C03C10/0072C03B32/02
Inventor D·L·J·达菲C·L·菲埃诺J·M·霍尔金宇辉V·M·施奈德
Owner CORNING INC
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