# US 2014/0193643 A1 · High Temperature Substrate Attachment Glass

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- Number: US 2014/0193643 A1
- Document ID: US20140193643A1
- Status: Published application
- Kind: A1
- Application number: 14/147,524
- Filed: 2014-01-04
- Published: 2014-07-10
- Earliest claimed: 2013-01-04
- Assignees: Lilliputian Systems, Inc.
- Applicants: Lilliputian Systems, Inc.
- Inventors: Mohammad Masyood Akhtar; Samuel B. Schaevitz; Michael C. Bradford; Zachary Byars; Joseph C. Tucker
- Web page: https://patentgrep.com/patent/US20140193643A1

## CPC

- B32B 17/06: comprising glass as the main or only constituent of a layer, next to another layer of a specific {material}
- B32B 17/00: Layered products essentially comprising sheet glass, or glass, slag, or like fibres
- C03C 3/066: containing zinc
- C03C 3/085: containing an oxide of a divalent metal
- C03C 3/093: containing zinc or zirconium
- C03C 8/24: Fusion seal compositions being frit compositions having non-frit additions, i.e. for use as seals between dissimilar materials, e.g. glass and metal; Glass solders
- C03C 10/0045: {containing SiO2, Al2O3 and MgO as main constituents}
- C03C 17/3618: {Coatings of type glass/inorganic compound/other inorganic layers, at least one layer being metallic}
- H01M 8/0282: Inorganic material
- Y02E 60/50: Fuel cells
- B32B: LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- C03C: CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- H01M: PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

A method of bonding a first substrate to a second substrate includes providing a glass, applying the glass in a layer between the first and second substrates to form an assembly, and heating the assembly to a bonding temperature above a glass transition temperature of the devitrifying glass, selected to cause the glass to bond the first substrate to the second substrate. The devitrifying glass has constituents that include various amounts of group A in a molar concentration of 70-95%, group B in a molar concentration of 5-20%, group C in a molar concentration of 1-20%, group D in a molar concentration of 0-6%; and group E in a molar concentration of 0-10%. The group A, B, C, D and E groups are disclosed herein.

## Claims

### Claim 1

A method of forming a glass, the method comprising:
providing ingredients;
heating ingredients together above a melting temperature to form a molten glass;
cooling the glass;
wherein the ingredients combine to provide constituents comprising:
group A in a molar concentration of 70-95%;
group B in a molar concentration of 5-20%;
group C in a molar concentration of 1-20%;
group D in a molar concentration of 0-6%;and
group E in a molar concentration of 0-10%;
wherein:
group A is selected from the group consisting of:
silicon oxides in a molar percent of 15-65%;
boron oxides in a molar percent of 0-20%;
zinc oxides in a molar percent of 15-55%;
phosphorous oxides in a molar percentage of 0-25%; and
combinations thereof;
group B is selected from the group consisting of:
aluminum oxides in a molar percent of 3-20%;
titanium oxides in a molar percent of 5-20%;
zirconium oxide in a molar percent of 5-20%;
yttrium oxide in a molar percent of 5-20%;and
combinations thereof;
group C is selected from the group consisting of:
magnesium oxides in a molar percent of 1-20%;
calcium oxides in a molar percent of 1-20%;
strontium oxides in a molar percent of 1-20%;
barium oxides in a molar percent of 1-20%; and
combinations thereof;
group D is selected the from the group consisting of:
titanium oxides in a molar percent of 0-6%;
zirconium oxides in a molar percent of 0-6%;
niobium oxides in a molar percent of 0-6%;
platinum in a molar percent of 0-6%;
manganese oxides in a molar percent of 0-6%;
cerium oxides in a molar percent of 0-6%; and
combinations thereof;
group E is selected from the group consisting of:
lithium in a molar percent of 0-10%;
sodium in a molar percent of 0-10%;
potassium in a molar percent of 0-10%;and
combinations thereof; and the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 2 (depends on 1)

A method according to claim 1, wherein cooling the glass includes placing molten glass in contact with a cooling material, the cooling material selected from the list water, a liquid with a boiling point below a crystallization temperature of the molten glass, a cooling substrate and combinations thereof.

### Claim 3 (depends on 1)

A method according to claim 1, wherein providing ingredients comprises ingredients that have a combined concentration of alkali oxides of less than 100 parts per million.

### Claim 4 (depends on 1)

A method according to claim 1, further comprising:
providing a first substrate and a second substrate;
applying the glass in a layer between the first and second substrates to form an assembly; and
heating the assembly to a bonding temperature, above a glass transition temperature of the devitrifying glass, selected to cause the glass to bond the first substrate to the second substrate.

### Claim 5 (depends on 4)

A method according to claim 4, wherein the glass has constituents comprising:
silicon oxides in a molar percent of 30-50%;
boron oxides in a molar percent of 0-10%;
zinc oxides in a molar percent of 25-45%;
aluminum oxides in a molar percent of 3-15%;
titanium oxides in a molar percent of 0-3%;
magnesium oxides in a molar percent of 10-20%; and combinations therefor:
and the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 6 (depends on 5)

A method according to claim 5, wherein the glass has constituents targeting a molar percentage comprising:
silicon oxides in a molar percent of 42-43%;
boron oxides in a molar percent of 4-5%;
zinc oxides in a molar percent of 33-35%;
aluminum oxides in a molar percent of 5-6%;
titanium oxides in a molar percent of 0.5-1%;
magnesium oxides in a molar percent of 12-13%; and combinations therefor:
and the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 7 (depends on 4)

A method according to claim 4, wherein one or both substrates are silicon.

### Claim 8 (depends on 4)

A method according to claim 4, wherein the glass is a devitrifying glass.

### Claim 9 (depends on 4)

A method according to claim 4, wherein the constituents of the glass are selected to cause the glass transition temperature to lie in a range between 550 and 800 degrees Centigrade.

### Claim 10 (depends on 4)

A method according to claim 4, wherein heating the assembly to a bonding temperature includes heating the assembly above a first crystallization temperature of the devitrifying glass so as to induce substantial crystallization of the glass.

### Claim 11 (depends on 4)

A method according to claim 4, wherein the constituents of the glass are selected to cause the first crystallization temperature of the glass to lie in a range between 700° C. and 1000° C.

### Claim 12 (depends on 4)

A method according to claim 4, further comprising:
while heating the assembly, also applying opposing forces to opposite sides of the assembly to increase density of the layer of devitrifying glass.

### Claim 13 (depends on 4)

A method according to claim 4, wherein applying the glass includes applying the glass as frit in a frit paste.

### Claim 14 (depends on 13)

A method according to claim 13, wherein the frit has an average particle size between about 5 and about 80 microns.

### Claim 15 (depends on 14)

A method according to claim 14, wherein the frit has a size distribution in the range between 0.5 um and 100 um.

### Claim 16 (depends on 12)

A method according to claim 12, wherein applying opposing forces is performed to achieve a density of the layer that is at least about 90%.

### Claim 17

A bonded assembly that withstands high temperatures comprising:
a first substrate;
a second substrate;
a glass, disposed between the two substrates and establishing a bond between the substrates, the glass comprising:
group A in a molar concentration of 70-95%;
group B in a molar concentration of 5-20%;
group C in a molar concentration of 1-20%;
group D in a molar concentration of 0-6%;and
group E in a molar concentration of 0-10%;
wherein:
group A is selected from the group consisting of:
silicon oxides in a molar percent of 15-65%;
boron oxides in a molar percent of 0-20%;
zinc oxides in a molar percent of 15-55%; and
combinations thereof;
group B is selected from the group consisting of:
aluminum oxides in a molar percent of 3-20%;
titanium oxides in a molar percent of 5-20%;
zirconium oxide in a molar percent of 5-20%;
yttrium oxide in a molar percent of 5-20%;and
combinations thereof; group C is selected from the group consisting of:
magnesium oxides in a molar percent of 1-20%;
calcium oxides in a molar percent of 1-20%;
strontium oxides in a molar percent of 1-20%;
barium oxides in a molar percent of 1-20%; and
combinations thereof;
group D is selected the from the group consisting of:
titanium oxides in a molar percent of 0-6%;
zirconium oxides in a molar percent of 0-6%;
niobium oxides in a molar percent of 0-6%;
platinum in a molar percent of 0-6%;
manganese oxides in a molar percent of 0-6%;
cerium oxides in a molar percent of 0-6%; and
combinations thereof;
group E is selected from the group consisting of:
lithium in a molar percent of 0-10%;
sodium in a molar percent of 0-10%;
potassium in a molar percent of 0-10%;and
the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 18 (depends on 17)

A bonded assembly of claim 17, wherein the glass has constituents comprising:
silicon oxides in a molar percent of 30-50%;
boron oxides in a molar percent of 0-10%;
zinc oxides in a molar percent of 25-45%;
aluminum oxides in a molar percent of 3-15%;
titanium oxides in a molar percent of 0-3%;
magnesium oxides in a molar percent of 10-20%; and combinations therefor:
and the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 19 (depends on 17)

A bonded assembly of claim 17,wherein the glass has constituents targeting a molar percentage comprising:
silicon oxides in a molar percent of 42-43%;
boron oxides in a molar percent of 4-5%;
zinc oxides in a molar percent of 33-35%;
aluminum oxides in a molar percent of 5-6%;
titanium oxides in a molar percent of 0.5-1%;
magnesium oxides in a molar percent of 12-13%; and combinations therefor:
and the foregoing percentages are expressed in relation to the glass composition as a whole.

### Claim 20 (depends on 17)

A bonded assembly of claim 17, wherein one or both substrates are silicon.

### Claim 21 (depends on 17)

A bonded assembly of claim 17, wherein the glass is a devitrifying glass.

### Claim 22 (depends on 17)

A bonded assembly of claim 17, wherein the bond between the first substrate and the second substrate is a hermetic seal between the substrates.

### Claim 23 (depends on 17)

A bonded assembly of claim 17, wherein composition is as the glass component in a frit paste.

### Claim 24 (depends on 23)

A bonded assembly of claim 23 where the average glass particle size is between 5 um and 80 um.

### Claim 25 (depends on 24)

A bonded assembly of claim 24, wherein the frit has a size distribution in the range between 0.5 um and 100 um.

### Claim 26 (depends on 17)

A bonded assembly of claim 17 where the bonding glass has a glass transition temperature between 550° C. and 800° C., and a crystallization temperature between 50° C. and 200° C. greater than the transition temperature.