Patent Application
20240167316
Certain example embodiments are generally related to vacuum insulated devices such as vacuum insulating panels that may be used for windows or the like, and/or methods of making same.
Vacuum insulated panels are known in the art. For example, and without limitation, vacuum insulating panels are disclosed in U.S. Pat. Nos. 5,124,185, 5,657,607, 5,664,395, 7,045,181, 7,115,308, 8,821,999, 10,153,389, and 11,124,450, the disclosures of which are all hereby incorporated herein by reference in their entireties.
As discussed and/or shown in one or more of the above patent documents, a vacuum insulating panel typically includes an outboard substrate, an inboard substrate, a hermetic edge seal, a sorption getter, a pump-out port, and spacers (e.g., pillars) sandwiched between at least the two substrates. The gap between the substrates may be at a pressure less than atmospheric pressure to provide insulating properties. Providing a vacuum in the space between the substrates reduces conduction and convection heat transport, and thus provides insulating properties. For example, a vacuum insulating panel provides thermal insulation resistance by reducing convective energy between the two substrates, reducing conductive energy between the two transparent substrates, and reducing radiative energy with a low-emissivity (low-E) coating provided on one of the substrates. Vacuum insulating panels may be used in window applications (e.g., for commercial and/or residential windows), and/or for other applications such as commercial refrigeration and consumer appliance applications.
In certain example embodiments, there may be provided a vacuum insulating panel which may comprise: a first substrate; a second substrate; a plurality of spacers provided in a gap between at least the first and second substrates, wherein the gap is at pressure less than atmospheric pressure; a seal provided at least partially between at least the first and second substrates, wherein the seal may comprise a first seal layer; and wherein the first seal layer may comprise a first continuous seal layer portion comprising seal material that surrounds at least the gap as viewed from above, and a second continuous seal layer portion comprising seal material that also surrounds at least the gap as viewed from above, wherein the first and second continuous seal layer portions may be spaced apart from each other as viewed from above so that a space may be located between at least the first and second continuous seal layer portions.
In certain example embodiments, there may be provided a vacuum insulating panel which may comprise: a first glass substrate; a second glass substrate; a plurality of spacers provided in a gap between at least the first and second glass substrates, wherein the gap is at pressure less than atmospheric pressure; a seal provided at least partially between at least the first and second substrates, wherein the seal may comprise a first seal layer; wherein the first seal layer may comprise first and second substantially coplanar spaced apart seal layer portions each comprising seal material, wherein the first and second substantially coplanar seal layer portions may be spaced apart from each other so that a space is located between at least the first and second seal layer portions, and wherein the second seal layer portion may be located between at least first seal layer portion and the gap at pressure less than atmospheric pressure.
Technical advantage(s), for example, include one or more of: (a) improved insulative properties, including edge-of-glass performance; (b) may permit use of a smaller diameter laser beam(s) and/or lower power level(s) during firing and/or sintering of the seal to reduce induced transient thermal stress and/or micro-cracking of the ceramic sealing material; (c) may permit use of a smaller laser beam(s) and/or lower power level(s) during firing and/or sintering of the seal to reduce de-tempering of glass substrate(s); (d) may increase laser sintering speed compared to a single row edge seal by allowing use of a smaller laser beam(s) and/or lower power level(s); (e) desirable mechanical strength to pass asymmetric thermal stress testing such as due to satisfying a desirable cumulative seal width; (f) desirable mechanical strength and/or structure to obtain desired fragmentation cullet size for tempered glass safety testing under constrained edge conditions; and/or (g) provide desirable cross-sectional total width to improve hermiticity of the edge seal.
These and/or other aspects, features, and/or advantages will become apparent and more readily appreciated from the following description of various example embodiments, taken in conjunction with the accompanying drawings. Thicknesses of layers/elements, and sizes of components/elements, are not necessarily drawn to scale or in actual proportion to one another, but rather are shown as example representations. Like reference numerals may refer to like parts throughout the several views. Each embodiment herein may be used in combination with any other embodiment(s) described herein.
The following detailed structural and/or functional description(s) is/are provided as examples only, and various alterations and modifications may be made. The example embodiments herein do not limit the disclosure and should be understood to include all changes, equivalents, and replacements within ideas and the technical scope herein.
Hereinafter, certain examples will be described in detail with reference to the accompanying drawings. When describing various example embodiments with reference to the accompanying drawings, like reference numerals may refer to like components and a repeated description related thereto may be omitted.
Conventional insulated glass edge sealing systems and associated sintering and/or firing processes have shown it is possible to create a hermetically sealed vacuum insulating panel. However, conventional vacuum insulated glass perimeter sealing systems may suffer from one or more of the following drawbacks that hinder use of such products commercially: (1) significant de-tempering of the glass substrate(s) preventing or reducing a likelihood of the vacuum insulated panel meeting mandatory tempered glass safety codes due to overall reduction in the compressive surface stress across the device and/or the internal tensile stress; (2) significantly higher de-tempering rates around the periphery of the device relative to the center of the vacuum insulated panel resulting in a large compressive stress gradient that upon physical impact does not meet safety fragmentation requirements, due for example and without limitation at least to variations in resonant vibration frequencies; (3) lack of durability, for example due to thermally induced breakage or flaws from large asymmetric thermal stress across the unit and/or spacer induced cracks causing glass breakage; (4) lack of durability and/or hermiticity due to edge seal damage, cracks and/or flaws; (5) failures due to too much induced transient thermal stress; (6) significant thermal de-tempering of tempered glass resulting in higher unit breakage rates such as when installed in a final application; and/or (7) ceramic sealing glass-based edge seals having unfavorable edge of glass u-factor due to a thermal bridge between opposing substrates. Certain example embodiments herein may overcome at least one of these problems.
Referring to
When heat strengthened glass substrates 1 and/or 2 are used, the substrate(s) may be heat strengthened prior to firing/sintering of the main edge seal material 30 (e.g., via laser) to form the edge seal 3. When a vacuum insulated glass panel/unit has one tempered glass substrate and one heat strengthened substrate, the substrate(s) may be tempered (e.g., thermally or chemically tempered) and heat strengthened prior to firing/sintering of the main edge seal material 30 (e.g., via laser) to form the edge seal 3.
In various example embodiments, an example vacuum insulating panel 100, still referring to
A vacuum insulating panel 100 may also include a pump-out tube 12 used for evacuating the space 5 to a pressure(s) less than atmospheric pressure, where the elongated pump-out tube 12 may be closed/sealed after evacuation of the space/gap 5. Pump-out seal 13 may be provided around tube 12, and a cap 14 may be provided over the top of the tube 12 after it is sealed. Tube 12 may extend part way through the substrate 1, for example part way through a double countersink hole drilled in the substrate as shown in
The evacuated gap/space 5 between the substrates 1 and 2, in the vacuum insulating panel 100, is at a pressure less than atmospheric pressure. For example, after the edge seal 3 has been formed, the cavity 5 evacuated to a pressure less than atmospheric pressure, and the pump-out tube 12 closed/sealed, the gap 5 between at least the substrates 1 and 2 may be at a pressure no greater than about 1.0×10−2 Torr, more preferably no greater than about 1.0×10−3 Torr, more preferably no greater than about 1.0×10−4 Torr, and for example may be evacuated to a pressure no greater than about 1.0×10−6 Torr. The gap 5 may be at least partially filled with an inert gas in various example embodiments. In certain example embodiments, the evacuated vacuum gap/space 5 may have a thickness (in a direction perpendicular to planes of the substrates 1 and 2) of from about 100-1,000 μm, more preferably from about 200-500 μm, and most preferably from about 230-350 μm. Providing a vacuum in the gap/space 5 is advantageous as it reduces conduction and convection heat transport, so as to reduce temperature fluctuations inside buildings and the like, thereby reducing energy costs and needs to heat and/or cool buildings. Thus, panels 100 can provide high levels of thermal insulation.
Example low-emittance (low-E) coatings 7 which may be used in the vacuum insulating panel 100 are described in U.S. Pat. Nos. 5,935,702, 6,042,934, 6,322,881, 7,314,668, 7,342,716, 7,632,571, 7,858,193, 7,910,229, 8,951,617, 9,215,760, and 10,759,693, the disclosures of which are all hereby incorporated herein by reference in their entireties. Other low-E coatings may also, or instead, be used. A low-E coating 7 typically includes at least one IR reflecting layer (e.g., of or including silver, gold, or the like) sandwiched between at least first and second dielectric layer(s) of or including materials such as silicon nitride, zinc oxide, zinc stannate, and/or the like. A low-E coating 7 may have one or more of: (i) a hemispherical emissivity/emittance of no greater than about 0.20, more preferably no greater than about 0.04, more preferably no greater than about 0.028, and most preferably no greater than about 0.015, and/or (ii) a sheet resistance (Rs) of no greater than about 15 ohms/square, more preferably no greater than about 2 ohms/square, and most preferably no greater than about 0.7 ohms/square, so as to provide for solar control. In certain example embodiments, the low-E coating 7 may be provided on the interior surface of the glass substrate to be closest to the building exterior, which is considered surface two (e.g., see
In certain example embodiments, primer layers 31 and 32 may be of or include different material(s) compared to the main seal layer 30. Thus, the main seal layer 30 and primers 31 and 32 can be sintered/fired in different heating steps, in a manner which allows thermal tempering of the glass substrates 1 and 2 when sintering/heating the primers on the respective glass substrates, and which allows the main seal layer 30 to thereafter be sintered and bonded to the primers 31 and 32 via laser heating without significantly de-tempering the glass substrates 1 and 2. This advantageously results in more efficient processing, reduction in damage (e.g., micro-cracking, adhesive failure, cohesive failure, and/or significant de-tempering), and a more durable and longer lasting vacuum insulating panel with much of its temper strength retained allowing for example compliance with industry safety testing for bag impact and/or point impact fragmentation.
The edge seal 3, in certain example embodiments, may be located at an edge-deleted area (where the solar control coating 7 has been removed) of the substrate as shown in
The low-E coating 7 may be edge deleted around the periphery of the entire unit so as to remove the low-e coating material from the coated glass substrate. The low-E coating 7 edge deletion width (edge of glass to edge of low-E coating 7), in certain example embodiments, in at least one area may be from about 0-100 mm, with examples being no greater than about 6 mm, no greater than about 10 mm, no greater than about 13 mm, no greater than about 25 mm, with an example being about 16 mm. In certain example embodiments, there may be a gap between the primer seal layers 31 and 32 and/or main layer 30, and the low-E coating 7, of at least about 0.5 mm, more preferably a gap of at least about 0.5 mm, more preferably at least about 1.0 mm, so that the low-E coating 7 is not contiguous with the main seal layer 30 and/or the primer seal layers 31 and 32.
As shown in
a illustrate an example embodiment where the main seal layer 30 includes first seal layer portion 30a (having a width W1) and second seal layer portion 30b (having a width W2), spaced apart from each other via space/gap 37 having width WA, and where both seal layer portions 30a and 30b overlap primer layer 31 and primer layer 32. In this embodiment, the main seal layer 30 has different layer portions, but the primer layers 31 and 32 do not as they are each made up of a single continuous layer. In this embodiment, the primer layers 31 and 32 each overlap and cover the gap 37. In this example embodiment, the main seal layer 30 is broken up into two distinct continuous bands 30a and 30b that surround the low pressure space/gap 5 as viewed from above (e.g., see
While main seal layer 30 may be separated into two distinct spaced apart seal layer portions 30a and 30b as shown in
The use of multiple seal portions (e.g., 30a and 30b) for at least main seal layer 30, as shown in
It has been found that adjusting the width (as viewed from above and/or in cross-section) of the main seal layer 30, of the edge seal, can be technically advantageous. For example, by making the main seal layer 30 narrower (smaller or reduced overall width, including each layer portion 30a, 30b individually, or combined), induced transient thermal stress in the layer 30 (and possibly the glass substrate) can be reduced which allows one to realize fast production times in combination with reduced chances of micro-cracking of the edge seal and/or adhesive or cohesive delamination problems. Reduced width of the main seal layer 30 can also improve U-value/U-factor performance of panel 100. The figures, for example, illustrate that the main edge seal layer 30 has a width less than the width of one or both of the adjacent primer layers 31 and 32. For example, referring to
Adjusting the width (as viewed from above and/or in cross-section) of one or both of the primer layers 31 and/or 32 may be technically advantageous in certain example embodiments. For example, see the width “Wp” of the primer layer 32 in
In certain example embodiments, as viewed from above and/or in cross-section as shown in
In certain example embodiments, in the manufactured vacuum insulating panel 100, the main seal layer 30 of the edge seal 3 may have an average thickness of from about 30-180 μm, more preferably from about 30-120 μm, more preferably from about 40-100 μm, and most preferably from about 50-85 μm, with an example main seal layer 30 average thickness being from about 60-80 μm. In certain example embodiments, in the manufactured vacuum insulating panel 100, the primer layer 31 of the edge seal 3 may have an average thickness of from about 10-100 μm, more preferably from about 10-80 μm, more preferably from about 20-70 μm, and most preferably from about 20-55 μm, with an example primer layer 31 average thickness being about 45 μm. In certain example embodiments, in the manufactured vacuum insulating panel 100, the primer layer 32 (opposite the side from which the laser beam 40 is directed) of the edge seal 3 may have an average thickness of from about 80-240 μm, more preferably from about 100-220 μm, more preferably from about 120-200 μm, and most preferably from about 120-170 μm, with an example primer layer 32 average thickness being about 145 μm. In certain example embodiments, the thickness of the main seal layer 30 may be at least about 30 μm thinner (more preferably at least about 45 μm thinner) than the thickness of the primer seal layer 32, and may be at least about 10 μm thicker (more preferably at least about 20 μm, and more preferably at least about 30 μm thicker) than the thickness of the primer seal layer 31. In certain example embodiments, in the manufactured vacuum insulating panel 100, the overall average thickness of the edge seal 3 may be from about 150-330 μm, more preferably from about 200-310 μm, and most preferably from about 220-290 μm, with an example overall edge seal 3 average thickness being about 270 μm. In certain example embodiments, the respective thicknesses of each layer 30, 31, and 32 may be substantially the same (the same plus/minus 10%, more preferably plus/minus 5%) along the length of the edge seal 3 around the periphery of the entire panel 100.
In certain example embodiments, in the manufactured vacuum insulating panel 100, the ratio TM/TP1 of the thickness TM of the main seal layer 30 to the thickness TP1 of thin primer layer 31 may be from about 1.2 to 2.2, more preferably from about 1.4 to 2.0, and most preferably from about 1.5 to 1.9 (e.g., the ratio TM/TP1 is 1.78 when a primer layer 31 is 45 μm thick and the main seal layer 30 is 80 μm thick as shown in
In certain embodiments, the main layer 30 may be a double row (e.g., see
In certain embodiments, the main layer 30 may be a triple row (e.g., see
In various example embodiments, a double row design (e.g., see
Table 1A sets forth example ranges for various elements and/or compounds for this example tellurium (Te) oxide based main seal 30 material according to various example embodiments, for both mol % and weight %, prior to firing/sintering thereof and thus prior to hermetic edge seal 3 formation. In certain example embodiments, the main seal layer 30 may comprise mol % and/or wt. % of the following compounds in one or more of the following orders of magnitude: tellurium oxide>vanadium oxide>aluminum oxide, tellurium oxide>vanadium oxide>silicon oxide, tellurium oxide>vanadium oxide>aluminum oxide>magnesium oxide, and/or tellurium oxide>vanadium oxide>silicon oxide>magnesium oxide, before and/or after firing/sintering of the layer 30. It will be appreciated that other materials may be used together, or in place of, those shown below, and that the example percentages may be different in alternate embodiments.
Tellurium Vanadate based and/or inclusive glasses (including tellurium oxide and vanadium oxide), such as those in Table 1A, in certain example embodiments are ideally suited for the main seal functionality when utilizing laser irradiation for the firing/sintering of the main seal layer 30. The base main seal material may comprise tellurium oxide (e.g., a combination of TeO3, TeO3+1, and TeO4) and vanadium oxide (e.g., a combination of V2O5, VO2, and V2O3) per the weight % and/or mol % described in Table 1A. In certain example embodiments, it may be desirable to have a higher amount of tellurium oxide compared to vanadium oxide, in order to increase the material density in the sintered state and thus improve hermiticity of the seal. With respect to main seal material(s) in Table 1A for the main seal layer 30, the Te oxide (e.g., one or more of TeO4, TeO3, TeO3+1, and/or other stoichiometry(ies) involving Te and O) and V oxide (e.g., one or more of VO2, V2O5, V2O3, and/or other stoichiometry(ies) involving V and O) in the material may be made up of about the following stoichiometries before/after sintering as shown below in Table 1B (tellurium oxide stoichiometries prior to firing/sintering), Table 1C (tellurium oxide stoichiometries after firing/sintering), Table 1D (vanadium oxide stoichiometries prior to firing/sintering), Table 1E (vanadium oxide stoichiometries after firing/sintering), respectively, measured via XPS.
For example, the “Example” column in Table 1B indicates that 57% of the Te present in the material prior to sintering/firing was in an oxidation state of TeO4, 42% of the Te present in the material prior to sintering/firing was in an oxidation state of TeO3, and 1% of the Te present in the material prior to sintering/firing was in an oxidation state of TeO3+1. And the “Example” column in Table 1C indicates that after the laser firing/sintering of the main seal layer 30 just 14% of the Te present in the main seal layer 30 material was in an oxidation state of TeO4, but 81% of the Te present in the material was in an oxidation state of TeO3, and 5% of the Te present in the material prior to sintering/firing was in an oxidation state of TeO3+1. Accordingly, in certain example embodiments, it will be appreciated that the laser firing/sintering of the main seal layer 30 may cause much of the TeO4 to transform/convert into TeO3 and TeO3+1, which is advantageous because it increases the material's absorption in the near infrared (e.g., 808 or 810 nm for example, which may be used for the laser during sintering/firing) which provides for increased heating efficiency and reducing the chances of significantly de-tempering the glass substrate(s) due to improved heating efficiency during the firing/sintering.
In certain example embodiments, prior to firing/sintering, the material for the main seal layer 30 may include tellurium oxide with the following stoichiometry/oxidation state ratio(s) in terms of what oxidation state(s) are used by the Te in the material (e.g., see Table 1B): TeO4>TeO3>TeO3+1. But the laser sintering/firing of the main seal layer may then cause the Te stoichiometry ratios/states to change to the following during/after sintering/firing: TeO3>TeO4>TeO3+1, which is advantageous in vacuum insulating panels as discussed above. The TeO4 is a trigonal bipyramid structure, TeO3 is a trigonal pyramid structure, and TeO3+1 is a polyhedral structure. In certain example embodiments, due to optimized laser treatment for firing/sintering of the main seal layer as discussed herein, the TeO4 largely converts to TeO3 and marginally to TeO3+1 with increasing temperature with a concurrent increase in the number of Te═O sites resulting from cleavage within the network structure.
For example, the “Example” column in Table 1D indicates that 84% of the V present in the material prior to sintering/firing was in an oxidation state of V2O5, 15% of the V present in the material prior to sintering/firing was in an oxidation state of VO2, and 1% of the V present in the material prior to sintering/firing was in an oxidation state of V2O3. And the “Example” column in Table 1E indicates that after the laser firing/sintering of the main seal layer just 25% of the V present in the main seal layer 30 material was in an oxidation state of V2O5, but 63% of the V present in the material was in an oxidation state of VO2, and 12% of the V present in the material prior to sintering/firing was in an oxidation state of V2O3. The other columns in Tables 1B-1E represent the same, with different values as shown. Accordingly, in certain example embodiments, it will be appreciated that the laser firing/sintering of the main seal layer 30 may cause much of the V2O5 to transform/convert into VO2 and V2O3, which is advantageous because it increases the material's density and thus the hermiticity and durability of the seal (e.g., VO2 results in a more dense layer than does V2O5). In certain example embodiments, it is desirable to reduce the V2O5 content in the final sintered/fired state of the main seal 30 because the glass network becomes more closed with decreasing V2O5 concentration, e.g., due to the reduction of non-bridging oxygen resulting in a higher density seal which improves water/moisture resistance, mechanical strength (adhesive and cohesive), and/or hermeticity. The Tg of the main seal 30 material may also slightly increase with a reduction in V2O5.
Thus, from Tables 1B-1E and
This main seal material(s), or substantially the same material, may also be used for the pump-out tube seal 13, with or without a primer, in certain example embodiments, although other types of seals may also be used such as vanadium oxide based ceramic sealing glass or solder glass. Other compounds may also be provided in this main seal 30 material, including but not limited to, on a weight and/or mol basis, for example one or more of: 0-15% (more preferably 1-10%) tungsten oxide; 0-15% (more preferably 1-10%) molybdenum oxide; 0-60% (or 38-52%) zinc oxide; 0-15% (more preferably 0-10%) copper oxide, and/or other elements shown in the figures.
Table 2 sets forth example ranges for various elements and/or compounds for this example tellurium oxide-based material for main seal layer 30 according to various example embodiments, for both mol and weight %, after firing/sintering thereof and thus after hermetic edge seal 3 formation. It will be appreciated that other materials may be used together, or in place of, those shown below, and that the example percentages may be different in alternate embodiments.
In certain example embodiments, the material for the main seal layer 30 may include filler. The filler may, for example, comprise one or more of zirconyl phosphates, dizirconium diorthophosphates, zirconium tungstates, zirconium vanadates, aluminum phosphate, cordierite, eucryptite, ekanite, alkaline earth zirconium phosphates such as (Mg,Ca,Ba,Sr) Zr4 P5O24, either alone or in combination. Filler in a range of 20-25 wt. % may be used in layer 30 in certain example embodiments. Main seal layer 30, and/or the primer layer(s) 31 and/or 32, is/are lead-free and/or substantially lead-free in certain example embodiments.
Table 3 sets forth example ranges for various elements for this example tellurium oxide based main seal 30 material according to various example embodiments, using elemental analysis (non-oxide analysis) for both mol % and weight %, prior to firing/sintering thereof and thus prior to hermetic edge seal 3 formation.
This material may also be used for the pump-out seal 13, with or without a primer, in certain example embodiments, although other types of seals may also be used such as vanadium oxide based ceramic sealing glass or solder glass. Other compounds may also be provided in this material (e.g., see
Table 4 sets forth example ranges for various elements for this example tellurium oxide based main seal 30 material according to various example embodiments, using elemental analysis (non-oxide analysis) for both mol % and weight %, after firing/sintering thereof and thus after formation of the hermetic edge seal 3 (e.g., see also
1-6%
This material may also be used for the pump-out seal 13, with or without a primer, in certain example embodiments, although other types of seals may also be used such as vanadium oxide based ceramic sealing glass or solder glass. Other compounds may also be provided in this material (e.g., see
Table 5 sets forth example ranges for various elements and/or compounds for this example primer material, for one or both layers 31 and/or 32, according to various example embodiments, for both mol % and weight %, prior to firing/sintering. In certain example embodiments, one or both of the primer layers 31 and/or 32 may comprise mol % and/or wt. % of the following compounds in one or more of the following orders of magnitude: boron oxide>bismuth oxide>silicon oxide, bismuth oxide>silicon oxide>boron, boron oxide>bismuth oxide>silicon oxide>titanium oxide, bismuth oxide>silicon oxide>boron oxide>titanium oxide, boron oxide>silicon oxide>titanium oxide>bismuth oxide, and/or silicon oxide>boron oxide>bismuth oxide, before and/or after formation of the hermetic edge seal 3. It will be appreciated that other materials may be used together, or in place of, those shown below, and that the example percentages may be different in alternate embodiments.
It is noted that “stoichiometry” as used herein covers, for example, oxygen coordination and oxygen state. Other compounds may also be provided in the primer material (e.g., see
Table 6 sets forth example ranges for various elements and/or compounds for this example primer layer 31 and/or 32 material according to various example embodiments, for both mol % and weight %, after firing/sintering thereof and after hermetic edge seal 3 formation. It will be appreciated that other materials may be used together, or in place of, those shown below, and that the example percentages may be different in alternate embodiments.
Other compounds may also be provided in this primer material, as discussed above and/or shown in the figures. Certain elements may change during firing/sintering, and certain elements may at least partially burn off during processing prior to formation of the final edges seal 3. It will be appreciated that, as with other layers discussed herein, other materials may be used together, or in place of, those shown above and/or below, and that the example weight/mol percentages may be different in alternate embodiments. The ceramic sealing glass primer materials for layer(s) 31 and/or 32 are lead-free and/or substantially lead-free in certain example embodiments.
Table 7 sets forth example ranges for various elements for the example primer material according to various example embodiments, using elemental analysis (non-oxide analysis) for both mol % and weight %, after firing/sintering thereof and thus after hermetic edge seal 3 formation.
The primer materials in
In certain example embodiments, main seal layer 30, after edge seal formation (e.g., via laser sintering), may have a density of at least about 2.75 g/cm3, more preferably of at least about 2.80 g/cm3, more preferably of at least about 2.90 g/cm3, more preferably of at least about 3.00 g/cm3, even more preferably of at least about 3.10 g/cm3, and most preferably of at least about 3.20 g/cm3. In certain example embodiments, the main seal layer 30, after edge seal formation (e.g., via laser sintering), may have a density of from about 2.80-4.00 g/cm3, more preferably from about 2.90-3.90 g/cm3, and most preferably from about 3.10-3.70 g/cm3 or 3.15-3.40 g/cm3. In certain example embodiments, these main seal layer 30 density ranges, preferably with a substantially lead-free ceramic material, may be in combination with a maximum processing temperature of the main seal layer 30 (e.g., during sintering and formation of the edge seal) during edge seal formation of no more than about 520 degrees C., more preferably no more than about 500 degrees C., and most preferably no greater than about 480 degrees C. For example, the main seal layer 30 may be of or include a material characterized by the above density ranges, after being processed at about 405 degrees C. for about 15 minutes. As explained above, such high densities advantageously provide for less porosity, good water resistance, good mechanical adhesion strength, and good hermiticity for the edge seal.
In certain example embodiments, one or both primer layer(s) 31 and/or 32 may have, after edge seal formation (e.g., via laser sintering), a density of at least about 2.75 g/cm3, more preferably of at least about 3.20 g/cm3, more preferably of at least about 3.40 g/cm3, more preferably of at least about 3.50 g/cm3, even more preferably of at least about 3.60 g/cm3. In certain example embodiments, one or both primer layers may have a density higher than the density of the main seal layer 30. The high density of the primer layer(s) is advantageous for improving hermiticity of the overall edge seal. In certain example embodiments, primer layer 31 and/or primer layer 32 may have a density of from about 3.0-4.2 g/cm3, more preferably from about 3.3-4.0 g/cm3, more preferably from about 3.5-3.8 g/cm3, more preferably from about 3.6-3.7 g/cm3. In certain example embodiments, primer layer 31 and/or primer layer 32 may have a density of at least about 0.20 g/cm3 higher (more preferably at least about 0.30 higher, more preferably at least about 0.40 higher) than a density of the main seal layer 30. For example, the main seal layer 30 may have a density of about 3.22 g/cm3 and the primer layers 31 and 32 may each have a density of about 3.66 g/cm3.
A substrate (e.g., substrate 1 in
In certain example embodiments, in steps 203 and 208, the primer layers 31 and 32 may bond to and/or diffuse into the respective glass substrates upon which they are located since the glass substrates 1, 2 are above the glass softening point, and create a high adhesion strength to the glass substrates. Interdiffusion of the primer layer(s) into the respective glass substrate(s) results in a high adhesion strength to the glass substrates, as for example SiO2 in the primer layer(s) bond to a silicon-rich layer in a soda lime silicate float glass in certain example embodiments. For example, adhesion strength using lap shear mechanical test methods may be from about 60-120 kg per cm2, which is higher than the modulus of rupture of soda lime silicate glass substrates. The primer layers may have a high degree of hermeticity, e.g., less than 1×10−8 cc/m2/day of vacuum loss, low moisture vapor transmission rates, and/or provide high levels of mechanical adhesion to the glass substrates, in certain example embodiments.
In step 204, the ceramic sealing glass main layer 30 (e.g., which may be Te oxide based or inclusive, or other suitable material) may then applied to one of the glass substrates over the primer layer (e.g., over primer 31, and/or over primer 32), such as via silkscreen printing, ceramic spray, extrusion coating, digital printing, pad printing, nozzle dispense or other commercially available ceramic sealing material application methods. The layer 30 may have tellurium oxide as a material with the highest weight percentage and vanadium oxide as a material with the second highest weight percentage, in certain example embodiments. The main seal layer 30 may then be thermally dried to remove solvents in the sealing glass matrix. The substrate may be thermally heated to remove solvents in the material using one of the following substrate heating methods or a combination thereof, radiation, convection, induction, microwave and/or conduction.
After the spacers are provided on a substrate in step 209, the two glass substrates 1 and 2 may then be mated together and clamped around the periphery of the vacuum insulated unit to create a mated unit in step 210. The pump-out tube 12 and preform 13 may be applied to the substrate having recess 15 between steps 210 and 211 in certain example embodiments. The mated unit may then be thermally heated to burn out the resin binders that provide the carrier vehicle for the sealing glass paste material and then pre-glazed at a temperature of about 370 degrees C. to impart mechanical strength properties and performance between the main layer and primer layer(s). For example, the perimeter of the vacuum insulated glass unit may be physically clamped with a controlled pressure to assist in setting the final thickness/height of the edge seal 3. The substrates may then be thermally heated to remove organic resin materials in the main sealing glass material 30 using one of the following substrate heating methods or a combination thereof; radiation, convection, induction, microwave or conduction. The binder burnout duration may be optimized so that much or substantially all binder is removed from the main layer 30 and the target density and/or porosity may be achieved. The mated unit may be heated between 250 degrees C. to 350 degrees C. for 30 seconds to twenty minutes with an example material temperature of 320 degrees C. and a duration of 8 minutes, in certain example embodiments; and/or heated between 340 degrees C. to 390 degrees C. for 30 seconds to ten minutes with an example material temperature of 370 degrees C. and a duration of 8 minutes. The mated unit may be heated to about 370 degrees C. to pre-glaze the main layer 30 in certain example embodiments. The pre-glaze may one or more of: (1) create a strong mechanical bond between the primer layer(s) and the main seal layer; (2) the main seal layer may reach or substantially reach its target thickness so the mechanical clamps may be removed prior to laser sintering; and/or (3) reduce process requirements for the laser to enable high linear rates.
In step 211, the mated unit may then be pre-heated to an ambient temperature of about 320 degrees C. (e.g., see pre-heating discussion above). The mated unit can be pre-heated using radiation, convection and/or conduction for example, with an example being a precision hot plate incorporating convective heating to achieve desired thermal uniformity across the substrate surfaces. The mated pair may be heated to 320 degrees C. to minimize or reduce the thermal delta between the glass substrate temperature and the sintering/melting point of the main seal layer 30 (e.g., which may be from about 390 degrees C. to 410 degrees C.) in certain example embodiments, so as to reduce transient thermal stress in the sealing glass materials. For example, transient thermal stress may be about 50 MPa without pre-heating to raise the ambient substrate temperature versus less than 10 MPa with pre-heating the glass substrates to about 320 degrees C.
In step 212, a laser (e.g., an 800 nm, 808 nm, 810 nm, or 940 nm continuous wave laser) 41 may then be used to locally and selectively sinter/fire the main seal layer 30. For example, the laser 41 and/or laser beam 40 may move around the periphery of the vacuum insulated unit using an XYZ gantry robot at a defined linear rate to wet the interface between the fully sintered primer layers 31, 32 and the pre-glazed main seal layer 30, sinter the main seal layer 30 to its final state (e.g., thickness, density and porosity) and to melt or partially melt the material to reduce the size of air pores in the main seal layer 30 and/or at the main layer to primer interface. The laser linear speed, laser power, laser beam size, laser irradiation time, and/or laser thermal decay time may be optimized to achieve desired physical, chemical and/or mechanical properties. The seal 13 around the pump-out tube 12 may be laser sintered/fired using the same or a different laser. In various example embodiments, a continuous wave 808-nm or 810-nm laser may be used to one or more of: (1) wet the surface or interface between the thin primer layer 31 and main seal layer 30 and the thick primer layer 32 and the main seal layer 30 to achieve for example a target 40 kg/cm2 mechanical adhesion; (2) locally sinter/fire the main seal layer 30 to densify material; and/or (3) locally melt the main layer material to fill in air voids/pores at the main seal layer 30 to primer layer(s) interface(s) that were generated during the main seal layer application process. While any type of laser may be used in various embodiments for sintering layer 30, a continuous wave laser may be preferred over a scanning/rastering laser scanning lasers may involve multiple pulses at a given irradiation spot resulting in a series of heating and cooling events that can increase transient stress and raise the final residual stress, which could result in micro-cracks that result in no or poor hermeticity.
In step 213, the space/gap 5 of the vacuum insulating panel is then evacuated to a low pressure using the pump-out tube 12, the tube closed off, and a cap 14 may be applied thereto.
In an example embodiment, there may be provided a vacuum insulating panel (e.g., 100) comprising: a first substrate (e.g., 1 or 2); a second substrate (e.g., 1 or 2); a plurality of spacers (e.g., 4) provided in a gap (e.g., 5) between at least the first and second substrates, wherein the gap (e.g., 5) is at pressure less than atmospheric pressure; a seal (e.g., 3) provided at least partially between at least the first and second substrates, the seal comprising a first seal layer (e.g., 30); and wherein the first seal layer (e.g., 30) comprises a first continuous seal layer portion (e.g., 30a) comprising seal material that surrounds at least the gap (e.g., 5) as viewed from above, and a second continuous seal layer portion (e.g., 30b) comprising seal material that also surrounds at least the gap as viewed from above, wherein the first and second continuous seal layer portions (e.g., 30a and 30b) are spaced apart from each other as viewed from above so that a space (e.g., 37) is located between at least the first and second continuous seal layer portions.
In the vacuum insulating panel of the immediately preceding paragraph, the first and second continuous seal layer portions may be concentric as viewed from above.
In the vacuum insulating panel of any of the preceding two paragraphs, the first and second continuous seal layer portions may be substantially rectangular in shape as viewed from above.
In the vacuum insulating panel of any of the preceding three paragraphs, the first continuous seal layer portion may surround the second continuous seal layer portion as viewed from above.
In the vacuum insulating panel of any of the preceding four paragraphs, the first and second continuous seal layer portions may be in a common plane.
In the vacuum insulating panel of any of the preceding five paragraphs, the first and second continuous seal layer portions may be substantially parallel to each other along at least part of at least one side of the panel.
In the vacuum insulating panel of any of the preceding six paragraphs, the first and second continuous seal layer portions may each comprise from about 40-70 wt. % tellurium oxide.
In the vacuum insulating panel of any of the preceding seven paragraphs, the first and second continuous seal layer portions may each comprise tellurium oxide and vanadium oxide, and by wt. % comprise more tellurium oxide than vanadium oxide.
In the vacuum insulating panel of any of the preceding eight paragraphs, from about 60-95% of Te in each of the first and second continuous seal layer portions may be in a form of TeO3, and from about 3-35% of Te in each of the first and second continuous seal layer portions may be in a form of TeO4. Tellurium oxide of the first seal layer may further comprise TeO3+1, and wherein each of the first and second continuous seal layer portions may comprise more TeO3 than TeO3+1 by wt. %. A ratio TeO4:TeO3 in each of the first and second continuous seal layer portions may be from about 0.05 to 0.40.
In the vacuum insulating panel of any of the preceding nine paragraphs, the first seal layer may comprise vanadium oxide which may comprise VO2 and V2O5, and wherein more V in each of the first and second continuous seal layer portions may be in a form of VO2 than V2O5. From about 35-85% of V in each of the first and second continuous seal layer portions may be in a form of VO2. From about 50-75% of V in each of the first and second continuous seal layer portions may be in a form of VO2. From about 5-45% of V in the each of the first and second continuous seal layer portions may be in a form of V2O5. The vanadium oxide may further comprise V2O3, and wherein more V in each of the first and second continuous seal layer portions may be in a form of VO2 than V2O3.
In the vacuum insulating panel of any of the preceding ten paragraphs, the seal may further comprise a second seal layer (e.g., primer layer) overlapping at least one of the first and second continuous seal layer portions. The second seal layer may comprise from about 30-60 mol % boron oxide; and/or may comprise from about 1-20 mol % bismuth oxide and from about 20-65 mol % boron oxide and comprises at least two times more boron oxide than bismuth oxide in terms of mol %. The second seal layer may comprise more boron oxide than bismuth oxide in terms of wt. %.
In the vacuum insulating panel of any of the preceding eleven paragraphs, the first seal layer may have a density of from about 2.8-4.0 g/cm3, and/or the second seal layer may have a density of from about 3.0-4.2 g/cm3, and wherein the density of the second seal layer may be at least about 0.20 g/cm3 greater than the density of the first seal layer.
In the vacuum insulating panel of any of the preceding twelve paragraphs, the first seal layer may be a main seal layer, and the second seal layer may be a primer layer. The second seal layer may comprise a first continuous seal layer primer portion that surrounds at least the gap as viewed from above, and a second continuous seal layer primer portion that also surrounds at least the gap as viewed from above, wherein the first and second continuous seal layer primer portions may be spaced apart from each other as viewed from above so that a space may be located between at least the first and second continuous seal layer primer portions.
In the vacuum insulating panel of any of the preceding thirteen paragraphs, the seal may further comprise a third seal layer (e.g., primer layer) overlapping at least one of the first and second continuous seal layer portions. The third seal layer may comprise from about 1-20 mol % bismuth oxide and/or from about 20-65 mol % boron oxide, and may comprise at least two times more boron oxide than bismuth oxide in terms of mol %. For at least one location of the seal, the first seal layer may have a first thickness, the second seal layer may have a second thickness, and the third seal layer may have a third thickness; and wherein the first thickness may be greater than the second thickness and less than the third thickness. For at least one location of the seal, a width of the first seal layer may be less than a width of the second seal layer by at least about 1 mm.
In the vacuum insulating panel of any of the preceding fourteen paragraphs, the seal may be substantially lead-free.
In the vacuum insulating panel of any of the preceding fifteen paragraphs, the first and second substrates may comprise glass substrates.
In the vacuum insulating panel of any of the preceding sixteen paragraphs, the first and second substrates may comprise tempered glass substrates or heat strengthened glass substrates.
In the vacuum insulating panel of any of the preceding seventeen paragraphs, the seal may be a hermetic edge seal of the vacuum insulating panel.
In the vacuum insulating panel of any of the preceding eighteen paragraphs, the panel may be configured for use in a window.
It is to be understood that a singular form of a noun corresponding to an item may include one or more of the things, unless the relevant context clearly indicates otherwise.
As used herein, “A or B”, “at least one of A and B”, “at least one of A or B”, “A, B or C”, “at least one of A, B and C”, and “A, B, or C,” each of which may include any one of the items listed together in the corresponding one of the phrases, or all possible combinations thereof. Terms such as “first”, “second”, or “first” or “second” may simply be used to distinguish the component from other components in question, and do not limit the components in other aspects (e.g., importance or order). Terms, such as “first”, “second”, and the like, may be used herein to describe various components. Each of these terminologies is not used to define an essence, order or sequence of a corresponding component but used merely to distinguish the corresponding component from other component(s). For example, a “first” component may be referred to as a “second” component, and similarly, the “second” component may be referred to as the “first” component. “Or” as used herein may cover both “and” and “or.”
It should be noted that if it is described that one component is “connected”, “coupled”, or “joined” to another component, at least a third component(s) may be “connected”, “coupled”, and “joined” between the first and second components, although the first component may be directly connected, coupled, or joined to the second component. Thus, terms such as “connected” and “coupled” cover both direct and indirectly connections and couplings.
The singular forms “a”, “an”, and “the” are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms “comprises/comprising” and/or “includes/including” when used herein, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components and/or populations thereof.
The word “about” as used herein means the identified value plus/minus 5%.
“On” as used herein covers both directly on, and indirectly on with intervening element(s) therebetween. Thus, for example, if element A is stated to be “on” element B, this covers element A being directly and/or indirectly on element B. Likewise, “supported by” as used herein covers both in physical contact with, and indirectly supported by with intervening element(s) therebetween.
Each embodiment herein may be used in combination with any other embodiment(s) described herein.
While the disclosure has been illustrated and described with reference to various example embodiments, it will be understood that the various embodiments are intended to be illustrative, not limiting. It will further be understood by those skilled in the art that various changes in form and detail may be made without departing from the true spirit and full scope of the disclosure, including the appended claims and their equivalents. It will also be understood that any of the embodiment(s) described herein may be used in combination with any other embodiment(s) described herein.
This application is related to and claims priority on U.S. Provisional Application No. 63/540,729, filed Sep. 27, 2023, the disclosure of which is hereby incorporated herein by reference in its entirety for all purposes. This application is also related to and claims priority on U.S. Provisional Application No. 63/427,645, filed Nov. 23, 2022, to U.S. Provisional Application No. 63/427,657, filed Nov. 23, 2022, and to U.S. Provisional Application No. 63/427,661, filed Nov. 23, 2022.
| Number | Date | Country | |
|---|---|---|---|
| 63540729 | Sep 2023 | US | |
| 63427645 | Nov 2022 | US | |
| 63427657 | Nov 2022 | US | |
| 63427661 | Nov 2022 | US | |
| 63427670 | Nov 2022 | US |
