WO2017155687A1 - Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant - Google Patents

Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant Download PDF

Info

Publication number
WO2017155687A1
WO2017155687A1 PCT/US2017/018782 US2017018782W WO2017155687A1 WO 2017155687 A1 WO2017155687 A1 WO 2017155687A1 US 2017018782 W US2017018782 W US 2017018782W WO 2017155687 A1 WO2017155687 A1 WO 2017155687A1
Authority
WO
WIPO (PCT)
Prior art keywords
microns
pillar
insulated glass
contact surface
structures
Prior art date
Application number
PCT/US2017/018782
Other languages
English (en)
Inventor
Margaret M. Vogel-Martin
Jeremy K. Larsen
Graham M. Clarke
Original Assignee
3M Innovative Properties Company
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 3M Innovative Properties Company filed Critical 3M Innovative Properties Company
Publication of WO2017155687A1 publication Critical patent/WO2017155687A1/fr

Links

Classifications

    • E—FIXED CONSTRUCTIONS
    • E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
    • E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
    • E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
    • E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
    • E06B3/663—Elements for spacing panes
    • E06B3/66304—Discrete spacing elements, e.g. for evacuated glazing units

Definitions

  • the present disclosure relates to pillars useful in insulated glass units (IGUs), particularly vacuum glazing, insulated glass units and insulated glass units containing the same
  • Pillars useful for insulated glass units have been described in, for example, U.S. Pat No. 6,479, 112 and U.S. Pat. Publ. No. 2010/0260950.
  • Double pane windows which include two glass panes with major surfaces substantially parallel to one another with a "space" or "gap" there between, are an improvement, as they provide a thermally insulating layer of gas, e.g. air, argon or the like, in the space between the window panes. Further improvement in a window's insulating capability can be achieved if the space between a double pane window is free of gas, i.e.
  • Windows of this type are often referred to as vacuum insulated glass units.
  • the pressure difference between the interior of the window and the exterior of the window may cause the glass panes to bow inward.
  • the bow is undesirable, as it adds undesirable stress to what generally are brittle materials, e.g. glass, and, in extreme cases, the window panes may contact one another, thereby reducing the thermal insulating effect of the evacuated gap.
  • manufactures have placed an array of small structures, often referred to as pillars, between the glass panels of a double pane window, to prevent the panels from bowing when vacuum is applied.
  • Windows with this array of pillars are referred to as vacuum insulated glazing units.
  • Window structures, including vacuum glazing have reduce the bow of the glass panels, with the addition of an array of pillars that supports the window panes and prevent the glass panels from bowing inward.
  • Vacuum glazing offers an improvement with respect to thermal insulation and the bowing of the glass panes is inhibited by the addition of an array of pillars.
  • the pillars create an additional problem.
  • the pillars have a higher thermal conductivity than the evacuated space between panes and each pillar creates a path of heat transfer between the two window panes that reduces the thermal insulating capability of the window.
  • the total surface area of the pillar and the individual pillars themselves are minimized, to minimize disruption of light propagation through the window and to minimize disruption of a viewer's view through the window.
  • the compressive stress transferred to the pillars from the glass panes may be high and the pillars may fracture, crack and/or deform under the applied load.
  • the pillars must have a suitably high compressive strength so as not to fail under the applied load.
  • the compressive stress the glass panes experience may be exacerbated at the edge of a pillar, as the edge, particularly a sharp edge, e.g. about a 90 degree angle between the face of the pillar contacting the glass and a corresponding pillar side-wall, may cause a stress concentration in the glass at the edge of the pillar.
  • Many current pillar designs currently employ a sharp pillar edge and may be prone to cause the glass to fracture due to stress concentration generated by the edges of the pillar.
  • the compressive stress on an individual pillar is increased and there is a greater tendency for the pillars to fail under the high loads.
  • the present disclosure provides new pillar designs that can lower thermal conductivity through the pillar, by reducing the contact area of the pillar with respect to the glass surfaces and/or improving the load bearing capabilities of the pillar and/or reducing stress concentration in the glass panes generated at the pillar edge. Additionally, if the pillar design includes an intricate structure, the design allows for fluid communication with the local environment throughout the pillar structure, preventing the trapping of undesirable gas within the pillar itself.
  • the present disclosure provides a pillar for use in a vacuum insulated glass unit comprising: a C-shaped body having a thickness, Tb, a first contact surface with first surface area Abl, an opposed second contact surface with second surface area Ab2, at least one sidewall, wherein the first contact surface comprises at least one first structure, integral with the first contact surface, the at least one first structure having a first structure base and a first structure face opposite the base, a thickness Tsl and a first structure face surface area, Asl .
  • the ratio of Tsl/Tb is between about 0.01 and about 0.6
  • the ratio of Asl/Abl is between about 0.03 and about 0.95 and/or the largest dimension of the body parallel to the first contact surface is between about 10 microns and about 2000 microns.
  • the at least one first structure may be a plurality of first structures. If a plurality of first structures is used, each of the individual first structures of the plurality of first structures has a first structure face opposite its base, each individual first structure face having a surface area asl .
  • the first structure face surface area, Asl may then be the sum of the first structure face surface area, asl, of each individual first structure of the plurality of first structures.
  • the opposed second contact surface of the C-shaped body may further comprise at least one second structure having a second structure base and a second structure face opposite the base, a thickness Ts2 and a second structure face surface area, As2.
  • the ratio of Ts2/Tb is between about 0.01 and 0.6 and/or the ratio of As2/Ab2 is between about 0.03 and about 0.95.
  • the at least one second structure may be a plurality of second structures. If a plurality of second structures is used, each of the individual second structures of the plurality of second structures has a second structure face opposite its base, each individual second structure face having a surface area as2.
  • the second structure face surface area, As2 may then be the sum of the second structure face surface area, as2, of each individual second structure of the plurality of second structures.
  • the C-shaped body is an annular segment shaped body.
  • the annular segment shaped body may include a segment angle theta ( ⁇ ), wherein theta is between about 150 degrees and about 355 degrees.
  • FIG. 1 A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. IB is a schematic front view of the exemplary pillar of FIG. 1 A according to one exemplary embodiment of the present disclosure.
  • FIG. 1C is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. ID is a schematic front view of the exemplary pillar of FIG. 1C according to one exemplary embodiment of the present disclosure.
  • FIG. 2B is a schematic perspective view of the exemplary pillar of FIG. 2 A according to one exemplary embodiment of the present disclosure.
  • FIG. 3 A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 3B is a schematic perspective view of the exemplary pillar of FIG. 3 A according to one exemplary embodiment of the present disclosure.
  • FIG. 4A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 4B is a schematic perspective view of the exemplary pillar of FIG. 4 A according to one exemplary embodiment of the present disclosure.
  • FIG. 5A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 5B is a schematic perspective view of the exemplary pillar of FIG. 5 A according to one exemplary embodiment of the present disclosure.
  • FIG. 6A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 7A is a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 8A is an exploded perspective view of a vacuum insulated glass unit.
  • FIG. 8B is a side sectional view of a portion of a vacuum insulated glass unit.
  • FIG. 9A is an SEM image, top view, of an exemplary pillar according to one exemplary embodiment (Example 1) of the present disclosure.
  • FIG. 9B is an SEM image, perspective view, of the exemplary pillar of FIG. 9A according to one exemplary embodiment (Example 1) of the present disclosure.
  • contact area relates to the surface area of a pillar or pillars designed to be in contact with the surface of another substrate, e.g. glass panels of an insulated glass unit (IGU) or vacuum insulated glass unit (VIGU).
  • IGU insulated glass unit
  • VIGU vacuum insulated glass unit
  • insulate refers to thermally insulating characteristics, unless otherwise noted.
  • rounded means a smooth, continuous curve having a shape that is at least one of a portion of a circle or a portion of an ellipse.
  • the present disclosure relates to pillars useful in the fabrication of insulated glass units, particularly, vacuum insulated glass units.
  • the pillars of the present disclosure have reduced contact area which may be achieved by including structures within the contact surface of the pillars. This may lead to reduced thermal conductivity through the pillars and better overall insulating characteristics of a VIGU containing the pillars.
  • the pillars of the present disclosure include a body.
  • the body has a thickness, Tb, a first contact surface with first surface area Abl, an opposed second contact surface with second surface area Ab2 and at least one sidewall.
  • the at least one first structure may be a plurality of first structures. If a plurality of first structures is used, each of the individual first structures of the plurality of first structures has a first structure face opposite its base, each individual first structure face having a surface area asl .
  • the first structure face surface area, Asl may then be the sum of the first structure face surface area, asl, of each individual first structure of the plurality of first structures.
  • the opposed second contact surface of the body may further comprise at least one second structure having a second structure base and a second structure face opposite the base, a thickness Ts2 and a second structure face surface area, As2.
  • FIG. 1A a schematic top view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • FIG. 1A shows pillar 100-1 which includes body 101 (a C-shaped body in this exemplary embodiment), having a first contact surface 110a, with surface area Ab l (i.e. the projected area of the upper surface of C-shaped body 100-1), and an opposed second contact surface 110b, with surface area Ab2 (i.e. the projected area of the lower surface of C-shaped body 100-1, see FIG. IB) and at least one sidewall 120.
  • First contact surface 110a includes at least one first structure 150a integral with first contact surface 110a. At least one first structure 150a has a first structure face 152a.
  • First surface area Abl represents the projection of the shown major surface of the body and would include the surface area (circular area) of the at least one first structure 150a.
  • At least one first structure 150a has a first structure face surface area, Asl .
  • FIG. IB a schematic front view of the exemplary pillar of FIG. 1A, shows pillar 100-1 including body 101 having sidewalls 120, first contact surface 110a and second contact surface 110b.
  • Body 101 includes at least one first structure 150a having a first structure base 151a (represented by the imaginary dashed line) and a first structure face 152a opposite the base.
  • a first draft angle, al is defined as the angle between first contact surface 110a, e.g. a line parallel to first structure face 152a, and at least one sidewall 120.
  • a second draft angle, a2 is defined as the angle between second contact surface 110b (as depicted by the horizontal dashed line extended from second contact surface 110b) and at least one sidewall 120.
  • the first draft angle and the second draft angle may be congruent angles. In the embodiment of FIGS. 1 A and IB, draft angles al and a2 are each about 90 degrees.
  • a dimension, Ld is defined as the largest dimension of the body parallel to the first contact surface.
  • the interior of the body is in fluid communication with the local environment through the opening, N, in the C- shaped body and/or the open region between the at least one first structure 150a.
  • the body may have an exterior perimeter P, of length Lp.
  • the C-shaped body is an annular segment shaped body, as shown in FIGS 1 A and IB.
  • the annular segment shaped body may include a segment angle theta ( ⁇ ).
  • Segment angle theta may define the size of opening N.
  • a cord drawn between one end of the C-shaped body and the other end, may also define opening N, e.g. a cord drawn between points PI and P2.
  • the point "C" represents the center point of the circular, annular segment shaped body
  • Ri represents the interior radius
  • Re represents the exterior radius.
  • FIGS. 4A and 4B show a schematic top view and a schematic perspective view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • Pillar 100-5 has a C-shaped body that is an annular segment shaped body and is similarly described as the pillars of FIGS 1 A-ID. The ends of the body near the opening have sharp corners and the opening is smaller than the opening of the pillar of FIGS. 2A and 2B.
  • the top perimeter of the body has rounded edges.
  • FIGS. 5A and 5B show a schematic top view and a schematic perspective view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • Pillar 100-6 has a C-shaped body that is an annular segment shaped body and is similarly described as the pillars of FIGS 1 A-ID.
  • the ends of the body near the opening have rounded corners and the opening is larger than the opening of the pillar of FIGS. 2A and 2B.
  • FIGS. 7A and 7B show a schematic top view and a schematic perspective view of an exemplary pillar according to one exemplary embodiment of the present disclosure.
  • Pillar 100-8 has a C-shaped body that is an annular segment shaped body and is similarly described as the pillars of FIGS 1 A-ID. The ends of the body near the opening have rounded corners and the opening is smaller than the opening of the pillar of FIGS. 2A and 2B.
  • the at least one first structure, integral with the first contact surface, has been modified to be circular shaped.
  • the pillar body of the present disclosure may include at least one through hole.
  • the through hole shape may coincide with the general shape of the pillar body, however the through hole shape may be different from that of the shape of the pillar body.
  • the shape of the through hole is not particularly limited.
  • the shape of the through hole includes, but is not limited to, circular, ellipse, triangular, square, rectangular, hexagonal, octagonal and the like.
  • a dimension, Tw, is defined as the largest dimension of the through hole parallel to the first contact surface. Ld is as previously described.
  • the ratio of Tw/Ld may be between about 0.05 and about 0.95, between about 0.10 and about 0.95, between about 0.20 and about 0.95, between about 0.30 and about 0.95, between about 0.05 and about 0.90, between about 0.10 and about 0.90, between about 0.20 and about 0.90, between about 0.30 and about 0.90, between about 0.05 and about 0.80, between about 0.10 and about 0.95, between about 0.20 and about 0.80, between about 0.30 and about 0.80, between about 0.05 and about 0.70, between about 0.10 and about 0.70, between about 0.20 and about 0.70, or even between about 0.30 and about 0.70.
  • the number of through holes is not particularly limited and may be between about 1 and about 20, between about 1 and about 10 or even between about one and about 5.
  • the pillar body of the present disclosure may include at least one channel. Addition of at least one channel to the first contact surface and/or second contact surface of the pillar body reduces the overall contact surface of the pillar body, as the area of the first contact surface and/or second contact surface are reduced by the inclusion of the at least one channel. This design feature may lead to reduced thermal conductivity, i.e. improved insulating capabilities, of the pillars of the present disclosure. If, for example, the body is in the shape of an annulus, inclusion of at least one first channel may aid in the evacuation of gas from interior of the annulus, when the pillar is used in a VIGU.
  • the thickness i.e.
  • the at least one first and/or second channel may be linear along its length, i.e. a line, arced, curved, wavy, sinusoidal and the like. If more than one first channel is present, the first channels may intersect or may not intersect, e.g. parallel first channels. If more than one second channel is present, the second channels may intersect or may not intersect, e.g. parallel channels.
  • the length of the channel i.e. the longest dimension, may be between about 10 micron and about 2000 microns.
  • the width of the channel may be between about 1 microns and about 1000 microns.
  • the depth, of the channel may be between about 1 micron and about 1000 microns.
  • the ratio of Tc/Tb between about 0.01 and about 0.50.
  • Tsl/Tc and/or Ts2/Tc may be between about 0.01 and about 0.9.
  • draft angles al ' ' and a2" can be defined for the sidewalls of the plurality of at least one first channel and at least one second channel. The values of draft angles al " and a2" are the same as those disclosed for draft angles al and a2.
  • each sidewall has a first draft angle, al, and a second draft angle, a2.
  • the first draft angle, al, for each sidewall is defined as the included angle between the first contact surface and the adjoining sidewall (as depicted in FIGS. IB and ID).
  • the second draft angle, a2, for each sidewall is defined as the angle between the second contact surface (as depicted by the horizontal dashed line extended from the second contact surface of FIGS. IB and ID) and the adjoining sidewall.
  • the first draft angle and the second draft angle may be congruent angles.
  • al and/or a2 may be between about 90 degrees and about 135 degrees, between about 95 degrees and about 135 degrees, between about 100 degrees and about 135 degrees, 90 degrees and about 130 degrees, between about 95 degrees and about 130 degrees, between about 100 degrees and about 130 degrees, 90 degrees and about 120 degrees, between about 95 degrees and about 120 degrees, between about 100 degrees and about 120 degrees, 90 degrees and about 110 degrees, between about 95 degrees and about 110 degrees, or even between about 100 degrees and about 110 degrees. If al is greater than 90 degrees, the associated sidewall will be a tapered sidewall and the second contact surface is defined as having the larger projected surface area.
  • the structure dimensions are uniform.
  • the percent non-uniformity of at least one distance dimension corresponding to the size of the plurality of first and/or second structures, e.g. length, height, width of the face or width at the base is less than about 20%, less than about 15%, less than about 10%, less than about 8%), less than about 6% less than about 4%, less than about 3%, less than about 2%, less than about 1.5% or even less than about 1%.
  • the percent non-uniformity is the standard deviation of a set of values divided by the average of the set of values mulitplied by 100.
  • the standard deviation and average can be measured by known statistical techniques.
  • the standard deviation may be calculated from a sample size of at least 5 structures, at least 10 structures, at least 15 structures or even at least 20 structures, or even more.
  • the sample size may be no greater than 200 structures, no greater than 100 structures or even no greater than 50 structures.
  • the sample may be selected randomly from a single region on the body or from multiple regions on the body.
  • a precisely shaped body may still be considered precisely shaped, even though it may undergo some shrinkage related to curing, drying or other thermal treatments, e.g. calcinting or sintering, as it retains the general shape of the mole cavity from which it was original produced.
  • the width of at least one first and/or at least one second structures may be between about 10 microns and about 1500 microns, between about 10 microns and about 1250 microns, between about 10 microns and about 1000 microns, between about 10 microns and about 750 microns, between about 10 microns and about 500 microns, between about 10 microns and about 250 microns, between about 50 microns and about 1500 microns, between about 50 microns and about 1250 microns, between about 50 microns and about 1000 microns, between about 50 microns and about 750 microns, between about 50 microns and about 500 microns, between about 50 microns and about 250 microns, between about 100 microns and about 1500 microns, between about 100 microns and about 1250 microns, between about 100 microns and about 1000 microns, between about 100 microns and about 750 microns, between about 100 microns and about 500 microns, or even between about 100 microns and about
  • the thickness of the at least one first and/or at least one second structures may be between about 1 micron and about 500 microns, between about 1 micron and about 250 microns, between about 1 microns and about 100 microns, between about 1 microns and about 50 microns, between about 5 microns and about 500 microns, between about 5 microns and about 250 microns, between about 5 microns and about 100 microns, between about 5 microns and about 50 microns, between about 10 microns and about 500 microns, between about 10 microns and about 250 microns, between about 10 microns and about 100 microns between about 10 microns and about 50 microns, between about 15 microns and about 500 microns, between about 15 microns and about 250 microns, between about 15 micron and about 100 microns, between about 15 micron and about 50 microns, between about 20 microns and about 500 microns, between about 20 microns and about 250 microns, between about 20 microns and
  • the structures may all have the same heights, i.e. thickness, or the heights may vary, per design.
  • the percent non-uniformity of the height, i.e. thickness, of a plurality of first structures and/or a plurality of second structures may be between about 0.01 percent and about 10 percent, between about 0.01 percent and 7 percent, between about 0.01 percent and about 5 percent, between about 0.01 percent and 4 percent, between about 0.01 percent and 3 percent, between about 0.01 percent and 2 percent or even between about 0.01 percent and 1 percent.
  • the height, i.e. thickness, of at least about 10%, at least about 30%) at least about 50%, at least 70%, at least about 80%>, at least about 90%, at least about 95%) or even at least about 100%> of a plurality of first and/or a plurality of second structures may be between about 1 micron and about 500 microns, between about 1 micron and about 250 microns, between about 1 micron and about 100 microns, between about 1 micron and about 50 microns, between about 5 microns and about 500 microns, between about 5 microns and about 250 microns, between about 5 microns and about 100 microns, between about 5 microns and about 50 microns, between about 10 microns and about 500 microns, between about 10 microns and about 250 microns, between about 10 microns and about 100 microns between about 10 microns and about 50 microns, between about 15 microns and about 500 microns, between about 15 microns and about 250 microns, between
  • the plurality of first and/or second structures may be uniformly distributed, i.e. have a single areal density, across the first contact surface of the body and second contact surface of the body, respectively, or may have different areal density across the first contact surface of the body and second contact surface of the body, respectively.
  • the areal density of the plurality of first and or second structures may be between about 10/mm 2 to about 100000/mm 2 , between about 10/mm 2 to about 75000/mm 2 , between about 10/mm 2 to about 50000/mm 2 , between about 10/mm 2 to about 30000/mm 2 , between about 50/mm 2 to about 100000/mm 2 , between about 50/mm 2 to about 750000/mm 2 , between about 50/mm 2 to about 50000/mm 2 , between about 50/mm 2 to about 30000/mm 2 , between about 100/mm 2 to about 100000/mm 2 , between about 100/mm 2 to about 75000/mm 2 , between about 100/mm 2 to about 50000/mm 2 , or even between about 100/mm 2 to about 30,000/mm 2 .
  • the plurality of first and/or second structures may be arranged randomly across the first and /or second contact surface, respectively, or may be arranged in a pattern, e.g. a repeating pattern, across the first and/or second contact surface, respectively.
  • Patterns include, but are not limited to, square arrays, hexagonal arrays and the like. Combination of patterns may be used.
  • draft angles ⁇ and ⁇ 2' can be defined for the sidewalls of the plurality of first and second structures.
  • the range in values of draft angles ⁇ and ⁇ 2' are the same as those disclosed for draft angles al and a2.
  • the ratio of the total area of the plurality of second structure faces, i.e. the sum of the area of the face of each structure, to the projected area of the second contact surface may be between about 0.10 to about 0.98, between about 0.10 to about 0.95, between about 0.10 to about 0.90, between about 0.10 and about 0.80, between about 0.01 and about 0.70, between about 0.20 to about 0.98, between about 0.20 to about 0.95, between about 0.20 to about 0.90, between about 0.20 and about 0.80, between about 0.20 and about 0.70, between about 0.30 to about 0.98, between about 0.30 to about 0.95, between about 0.30 to about 0.90, between about 0.30 and about 0.80, between about 0.30 and about 0.70, between about 0.40 to about 0.98, between about 0.40 to about 0.95, between about 0.40 to about 0.90, between about 0.40 and about 0.80, between about 0.40 and about 0.70, between about 0.50 to about 0.98, between about 0.50 to about 0.95, between about 0.10 to about 0.90,
  • the pillar bodies of the present disclosure may include a peripheral edge. In some embodiments, at least a portion of the peripheral edge is at least one of rounded and chamfered. Pillars having bodies which include rounded and/or chamfered peripheral edges, are discussed in commonly assigned U.S. Patent Application Ser. No. 62/132054, entitled “VACUUM GALZING PILLARS FOR INSULATED GLASS UNITS AND INSULATED GLASS UNITS THEREFROM", filed March 12, 2015, which is hereby incorporated herein by reference in its entirety. Pillars having bodies which include a plurality of structures on their surfaces and/or at least one channel are discussed in commonly assigned U.S. Patent Application Ser. No. 62/132073, entitled "VACUUM GALZING PILLARS FOR INSULATED GLASS UNITS AND INSULATED GLASS
  • the pillar bodies of the present disclosure may further include a microstructure texture.
  • the present disclosure provides a pillar for use in a vacuum insulated glass unit comprising a body, the body includes a first contact surface and an opposed second contact surface, wherein at least one of a portion of the first contact surface and/or a portion of the second contact surface includes a microstructure texture.
  • a portion of both the first contact surface and second contact surface include a microstructure texture.
  • one or both of the entire first contact surface and the entire second contact surface includes microstructure texture.
  • the present disclosure provides a pillar for use in a vacuum insulated glass unit comprising a body, the body includes a first contact surface and an opposed second contact surface, wherein the first contact surface includes a microstructure texture; and the second contact surface further includes at least one second structure, each second structure having a second structure face.
  • at least a portion of the second structure face include a microstructure texture.
  • all of the second structure faces include a microstmcture texture.
  • microstmcture texture Pillars which include microstmcture texture are discussed in commonly assigned U.S. Patent Application Ser. No. 62/132073, entitled “VACUUM GALZING PILLARS FOR INSULATED GLASS UNITS AND INSULATED GLASS UNITS THEREFROM", filed on March 12, 2015, which was previously incorporated herein by reference in its entirety.
  • the height of the microstmcture texture is less than the height of the at least one first stmcture and/or at least one second stmcture. In some embodiments, the height of the microstmcture texture is between about 5 nanometers to about 5 microns.
  • the microstmcture texture may be in random pattern. In some embodiments, the microstmcture texture may be in a pattern. In some embodiments, the length of microstmcture texture is less than the length of the at least one first stmcture and/or the at least one second stmcture. In some embodiments, the length of the microstmcture texture is between about 5 nanometers to about 5 microns. In some embodiments, the width of microstmcture texture is less than the width of the at least one first stmcture and/or at least one second. In some
  • the pillar body may be at least one of a continuous, inorganic material or a polymer composite.
  • a "continuous inorganic material” is an inorganic material that spans the entire length, width and height of the pillar body. Due to the applied loads the pillars must withstand, it is preferable that they have a high compressive strength.
  • the compressive strength of the pillar may be greater than about 400 MPa, greater than about 600 MPa, greater than about 800 MPa, greater than about 1
  • the compressive strength is between about 400 MPa and about 110 GPa, between about 400 MPa and about 50 GPa, between about 400 MPa and about 25 GPa, between about 400 MPa and about 12 GPa, 1 GPa and about 110 GPa, between about 1 GPa and about 50 GPa, between about 1 GPa and about 25 GPa, or even between about 1 GPa and about 12 GPa.
  • the pillar body may have a thermal conductivity of less than about 40 W m "2 °K _1 , less than 20 W m "2 °K _1 , less than 10 W m "2 °K _1 or even less than 5 W m "2 °K _1 .
  • the pillar body may have a thermal conductivity of at least 0.1 W m "2 °K _1 .
  • the continuous inorganic material includes a ceramic, such as alpha alumina, and is fabricated via the molding of a sol gel precursor (the "sol gel route").
  • Ceramics are often opaque in appearance due to the scattering of light by pores in the ceramic. In order to achieve even a limited level of translucency, the density of the ceramic is typically greater than 99% of theoretical. Higher clarity can require levels above 99.9% or even 99.99%.
  • Two methods known in the art for achieving very high densities in ceramic materials are hot isostatic pressing and spark plasma sintering.
  • the continuous inorganic material may be crystalline metal oxide wherein at least 70 mole percent of the crystalline metal oxide is Zr0 2 , wherein from 1 to 15 mole percent (in some embodiments 1 to 9 mole percent) of the crystalline metal oxide is Y 2 Cb, and wherein the Zr0 2 has an average grain size in a range from 75 nanometers to 400 nanometers.
  • the crystalline metal oxide may have a density of at least 98.5 (in some embodiments, 99, 99.5, 99.9, or even at least 99.99) percent of theoretical density.
  • the volume of unit cell is measured by XRD for each composition or calculated via ionic radii and crystal type.
  • Nc number of atoms in unit cell
  • Vc Volume of unit cell [m 3 ]
  • N a Avogadro's number [atoms/mol].
  • the pillar body is formed from a reaction mixture that includes (a) 20 to 60 weight percent zirconia-based particles based on a total weight of the reaction mixture, the zirconia-based particles having an average particle size no greater than 100 nanometers and containing at least 70 mole percent Zr0 2 , (b) 30 to 75 weight percent of a solvent medium based on the total weight of the reaction mixture, the solvent medium containing at least 60 percent of an organic solvent having a boiling point equal to at least 150°C, (c) 2 to 30 weight percent polymerizable material based on a total weight of the reaction mixture, the polymerizable material including (1) a first surface modification agent having a free radical polymerizable group; and (d) a photoinitiator for a free radical polymerization reaction.
  • the zirconia-based particles can contain 0 to 30 weight percent yttrium oxide based on the total moles of inorganic oxide present. If yttrium oxide is added to the zirconia-based particles, it is often added in an amount equal to at least 1 mole percent, at least 2 mole percent, or at least 5 mole percent. The amount of yttrium oxide can be up to 30 mole percent, up to 25 mole percent, up to 20 mole percent, or up to 15 mole percent.
  • the amount of yttrium oxide can be in a range of 1 to 30 mole percent, 1 to 25 mole percent, 2 to 25 mole percent, 1 to 20 mole percent, 2 to 20 mole percent, 1 to 15 mole percent, 2 to 15 mole percent, 5 to 30 mole percent, 5 to 25 mole percent, 5 to 20 mole percent, or 5 to 15 mole percent.
  • the mole percent amounts are based on the total moles of inorganic oxide in the zirconia-based particles.
  • the zirconia-based particles can contain 0 to 10 mole percent lanthanum oxide based on the total moles of inorganic oxide present. If lanthanum oxide is added to the zirconia-based particles, it can be used in an amount equal to at least 0.1 mole percent, at least 0.2 mole percent, or at least 0.5 mole percent. The amount of lanthanum oxide can be up to 10 mole percent, up to 5 mole percent, up to 3 mole percent, up to 2 mole percent, or up to 1 mole percent.
  • the amount of lanthanum oxide can be in a range of 0.1 to 10 mole percent, 0.1 to 5 mole percent, 0.1 to 3 mole percent, 0.1 to 2 mole percent, or 0.1 to 1 mole percent.
  • the mole percent amounts are based on the total moles of inorganic oxide in the zirconia-based particles.
  • the zirconia-based particles contain 70 to 100 mole percent zirconium oxide, 0 to 30 mole percent yttrium oxide, and 0 to 10 mole percent lanthanum oxide.
  • the zirconia-based particles contain 70 to 99 mole percent zirconium oxide, 1 to 30 mole percent yttrium oxide, and 0 to 10 mole percent lanthanum oxide.
  • the zirconia-based particles contain 85 to 95 mole percent zirconium oxide, 5 to 15 mole percent yttrium oxide, and 0 to 5 mole percent (e.g., 0.1 to 5 mole percent or 0.1 to 2 mole percent) lanthanum oxide.
  • the mole percent amounts are based on the total moles of inorganic oxide in the zirconia-based particles.
  • inorganic oxides can be used in combination with a rare earth element or in place of a rare earth element.
  • calcium oxide, magnesium oxide, or a mixture thereof can be added in an amount in a range of 0 to 30 weight percent based on the total moles of inorganic oxide present. The presence of these inorganic oxides tends to decrease the amount of monoclinic phase formed. If calcium oxide and/or magnesium oxide is added to the zirconia-based particles, the total amount added is often at least 1 mole percent, at least 2 mole percent, or at least 5 mole percent.
  • the amount of calcium oxide, magnesium oxide, or a mixture thereof can be up to 30 mole percent, up to 25 mole percent, up to 20 mole percent, or up to 15 mole percent.
  • the amount can be in a range of 1 to 30 mole percent, 1 to 25 mole percent, 2 to 25 mole percent, 1 to 20 mole percent, 2 to 20 mole percent, 1 to 15 mole percent, 2 to 15 mole percent, 5 to 30 mole percent, 5 to 25 mole percent, 5 to 20 mole percent, or 5 to 15 mole percent.
  • the mole percent amounts are based on the total moles of inorganic oxide in the zirconia-based particles.
  • aluminum oxide can be included in an amount in a range of 0 to less than 1 mole percent based on a total moles of inorganic oxides in the zirconia-based particles.
  • Some example zirconia-based particles contain 0 to 0.5 mole percent, 0 to 0.2 mole percent, or 0 to 0.1 mole percent of these inorganic oxides.
  • the reaction mixture (casting sol) used to form the gel composition typically contains 20 to 60 weight percent zirconia-based particles based on a total weight of the reaction mixture.
  • the amount of zirconia-based particles can be at least 25 weight percent, at least 30 weight percent, at least 35 weight percent, or at least 40 weight percent and can be up to 55 weight percent, up to 50 weight percent, or up to 45 weight percent.
  • the amount of the zirconia-based particles are in a range of 25 to 55 weight percent, 30 to 50 weight percent, 30 to 45 weight percent, 35 to 50 weight percent, 40 to 50 weight percent, or 35 to 45 weight percent based on the total weight of the reaction mixture used for the gel composition.
  • Suitable organic solvents that have a boiling point equal to 150°C are typically selected to be miscible with water, as the zirconia-based particles may be formed in a water base medium and the organic solvents may be added to the zirconia-based particle sol and the water removed through distillation, leaving the organic solvent in its place.
  • the solvent medium contains at least 70 weight percent, at least 80 weight percent, at least 90 weight percent, at least 95 weight percent, at least 97 weight percent, at least 98 weight percent, or at least 99 weight percent of the organic solvent having a boiling point equal to at least 150°C.
  • the boiling point is often at least 160°C, at least 170°C, at least 180°C, or at least 190°C
  • the organic solvent is often a glycol or polyglycol, mono-ether glycol or mono- ether polyglycol, di-ether glycol or di-ether polyglycol, ether ester glycol or ether ester polyglycol, carbonate, amide, or sulfoxide (e.g., dimethyl sulfoxide).
  • the organic solvents usually have one or more polar groups.
  • the organic solvent does not have a polymerizable group; that is, the organic solvent is free of a group that can undergo free radical polymerization. Further, no component of the solvent medium has a polymerizable group that can undergo free radical polymerization.
  • Suitable glycols or polyglycols, mono-ether glycols or mono-ether polyglycols, di- ether glycols or di-ether polyglycols, and ether ester glycols or ether ester polyglycols are often of Formula (I).
  • each R 1 independently is hydrogen, alkyl, aryl, or acyl.
  • Suitable alkyl groups often have 1 to 10 carbon atoms, 1 to 6 carbon atoms, or 1 to 4 carbon atoms.
  • Suitable aryl groups often have 6 to 10 carbon atoms and are often phenyl or phenyl substituted with an alkyl group having 1 to 4 carbon atoms.
  • Suitable acyl groups are often of formula -(CO)R a where R a is an alkyl having 1 to 10 carbon atoms, 1 to 6 carbon atoms, 1 to 4 carbon atoms, 2 carbon atoms, or 1 carbon atom.
  • the acyl is often an acetate group (-(CO)CH3).
  • each R 2 is typically ethylene or propylene.
  • the variable n is at least 1 and can be in a range of 1 to 10, 1 to 6, 1 to 4, or 1 to 3.
  • R is hydrogen or an alkyl such as an alkyl having 1 to 4 carbon atoms, 1 to 3 carbon atoms, or 1 carbon atom. Examples include ethylene carbonate and propylene carbonate.
  • group R 4 is hydrogen, alkyl, or combines with R 5 to form a five- membered ring including the carbonyl attached to R 4 and the nitrogen atom attached to R 5 .
  • Group R 5 is hydrogen, alkyl, or combines with R 4 to form a five-membered ring including the carbonyl attached to R 4 and the nitrogen atom attached to R 5 .
  • Group R 6 is hydrogen or alkyl. Suitable alkyl groups for R 4 , R 5 , and R 6 have 1 to 6 carbon atoms, 1 to 4 carbon atoms, 1 to 3 carbon atoms, or 1 carbon atom.
  • amide organic solvents of Formula (III) include, but are not limited to, formamide, ⁇ , ⁇ -dimethylformamide, N,N- dimethylacetamide, N,N-diethylacetamide, N-methyl-2-pyrrolidone, and N-ethyl-2- pyrrolidone.
  • the reaction mixture often includes at least 30 weight percent solvent medium. In some embodiments, the reaction mixture contains at least 35 weight percent, or at least 40 weight percent solvent medium.
  • the reaction mixture can contain up to 75 weight percent, up to 70 weight percent, up to 65 weight percent, up to 60 weight percent, up to 55 weight percent, up to 50 weight percent, or up to 45 weight percent solvent medium.
  • the reaction mixture can contain 30 to 75 weight percent, 30 to 70 weight percent, 30 to 60 weight percent, 30 to 50 weight percent, 30 to 45 weight percent, 35 to 60 weight percent, 35 to 55 weight percent, 35 to 50 weight percent, or 40 to 50 weight percent solvent medium.
  • the weight percent values are based on the total weight of the reaction mixture.
  • the solvent medium typically contains less than 15 weight percent water, less than 10 percent water, less than 5 percent water, less than 3 percent water, less than 2 percent water, less than 1 weight percent, or even less than 0.5 weight percent water after the solvent exchange (e.g., distillation) process.
  • the reaction mixture includes one or more polymerizable materials that have a polymerizable group that can undergo free radical polymerization (i.e., the polymerizable group is free radical polymerizable).
  • the polymerizable group is an ethylenically unsaturated group such as a (meth)acryloyl group, which is a group of formula where R b is hydrogen or methyl.
  • the polymerizable material is usually selected so that it is soluble in or miscible with the organic solvent having a boiling point equal to at least 150°C.
  • the reaction mixture includes one or more polymerizable materials that have a polymerizable group that can undergo free radical polymerization (i.e., the polymerizable group is free radical polymerizable).
  • the polymerizable group is an ethylenically unsaturated group such as a (meth)acryloyl group, which is a group of formula where R b is hydrogen or methyl.
  • the polymerizable material is usually selected so that it is soluble in or miscible with the organic solvent having a boiling point equal to at least 150°C.
  • the polymerizable material includes a first monomer that is a surface modification agent having a free radical polymerizable group.
  • the first monomer typically modifies the surface of the zirconia-based particles.
  • Suitable first monomers have a surface modifying group that can attach to a surface of the zirconia-based particles.
  • the surface modifying group is usually a carboxyl group (-COOH or an anion thereof) or a silyl group of formula -Si(R 7 )x(R 8 )3-x where R 7 is a non-hydrolyzable group, R 8 is hydroxyl or a hydrolyzable group, and the variable x is an integer equal to 0, 1, or 2.
  • Suitable non-hydrolyzable groups are often alkyl groups such as those having 1 to 10, 1 to 6, 1 to 4, or 1 to 2 carbon atoms.
  • Suitable hydrolyzable groups are often a halo (e.g., chloro), acetoxy, alkoxy group having 1 to 10, 1 to 6, 1 to 4, or 1 to 2 carbon atoms, or group of formula
  • R d is an alkylene having 1 to 4 or 1 to 2 carbon atoms and R e is an alkyl having 1 to 4 or 1 to 2 carbon atoms.
  • the first monomer can function as a polymerizable surface modification agent. Multiple first monomers can be used. The first monomer can be the only kind of surface modification agent or can be combined with one or more other non-polymerizable surface modification agents such as those discussed above. In some embodiments, the amount of the first monomer is at least 20 weight percent based on a total weight of polymerizable material. For example, the amount of the first monomer is often at least 25 weight percent, at least 30 weight percent, at least 35 weight percent, or at least 40 weight percent. The amount of the first monomer can be up to 100 percent, up to 90 weight percent, up to 80 weight percent, up to 70 weight percent, up to 60 weight percent, or up to 50 weight percent. Some reaction mixtures contain 20 to 100 weight percent, 20 to 80 weight percent, 20 to 60 weight percent, 20 to 50 weight percent, or 30 to 50 weight percent of the first monomer based on a total weight of polymerizable material.
  • polymerizable material typically contains 20 to 100 weight percent first monomer and 0 to 80 weight percent second monomer based on a total weight of polymerizable material.
  • polymerizable material includes 30 to 100 weight percent first monomer and 0 to 70 weight percent second monomer, 30 to 90 weight percent first monomer and 10 to 70 weight percent second monomer, 30 to 80 weight percent first monomer and 20 to 70 weight percent second monomer, 30 to 70 weight percent first monomer and 30 to 70 weight percent second monomer, 40 to 90 weight percent first monomer and 10 to 60 weight percent second monomer, 40 to 80 weight percent first monomer and 20 to 60 weight percent second monomer, 50 to 90 weight percent first monomer and 10 to 50 weight percent second monomer, or 60 to 90 weight percent first monomer and 10 to 40 weight percent second monomer.
  • the weight ratio of polymerizable material to zirconia-based particles is often at least 0.05, at least 0.08, at least 0.09, at least 0.1, at least 0.11, or at least 0.12.
  • the weight ratio of polymerizable material to zirconia-based particles can be up to 0.80, up to 0.6, up to 0.4, up to 0.3, up to 0.2, or up to 0.1.
  • the ratio can be in a range of 0.05 to 0.8, 0.05 to 0.6, 0.05 to 0.4, 0.05 to 0.2, 0.05 to 0.1, 0.1 to 0.8, 0.1 to 0.4, or 0.1 to 0.3.
  • the reaction mixtures advantageously are initiated by application of actinic radiation. That is, the polymerizable material is polymerized using a photoinitiator rather than a thermal initiator.
  • a photoinitiator rather than a thermal initiator tends to result in a more uniform cure throughout the gel composition ensuring uniform shrinkage in subsequent steps involved in the formation of sintered articles.
  • the outer surface of the cured part is more uniform and more defect free when a photoinitiator is used rather than a thermal initiator.
  • the photoinitators are selected to respond to ultraviolet and/or visible radiation. Stated differently, the photoinitiators usually absorb light in a wavelength range of 200 to 600 nanometers, 300 to 600 nanometers, or 300 to 450 nanometers.
  • Some exemplary photoinitiators are benzoin ethers (e.g., benzoin methyl ether or benzoin isopropyl ether) or substituted benzoin ethers (e.g., anisoin methyl ether).
  • Other exemplary photoinitiators are substituted acetophenones such as 2,2- diethoxyacetophenone or 2,2-dimethoxy-2-phenylacetophenone (commercially available under the trade designation IRGACURE 651 from BASF Corp.
  • photoinitiators are substituted alpha-ketols such as 2-methyl-2-hydroxypropiophenone, aromatic sulfonyl chlorides such as 2-naphthalenesulfonyl chloride, and photoactive oximes such as 1 -phenyl- l,2-propanedione-2-(0-ethoxycarbonyl)oxime.
  • Pillars may be monolithic or composite.
  • Composite pillars may comprise a high compressive strength sintered ceramic core and one or more functional layers.
  • the pillar body can be fabricated by a molding process.
  • the shape of the body is determined by the mold cavity used.
  • the mold cavity generally, having the inverse shape corresponding to and dimensions of the desired pillar body shape.
  • rounded and/or chamfered corners and rounded and/or chamfered edges may be included in the mold cavity (inverse shape), such that, the rounded and/or chamfered corners and rounded and/or chamfered edges may be integrally in the pillar body, when the body is formed.
  • the at least one first structure and/or at least one second structure (inverse shape) may be included in the corresponding region of the mold and the at least one first structure and/or at least one second structure may be integrally formed in the pillar body, when the body is formed.
  • One or more channels may be integrally formed using the same approach.
  • Monolithic pillar bodies can be made via continuous and discontinuous processes.
  • One such process is a sol gel process.
  • Sol gel processes are disclosed in pending U.S. Appl. No. 14/025958, titled "VACUUM GLAZING PILLARS FOR INSULATED GLASS UNITS", filed September, 13, 2013 and pending U.S. Provisional Appl. No. 62/127569, titled GEL COMPOSITIONS AND SINTERED ARTICLES PREPARED
  • THEREFROM filed March, 3, 2015, which has been incorporated herein in its entirety by reference.
  • This process involves molding of gel bodies from a reaction mixture on a continuous belt, drying, demolding, and sintering. This process may yield bodies with some asymmetry. Surfaces in contact with the mold during the fabrication side may be smoother than the surface with an air interface. In addition, samples may warp or cup slightly during drying to form a pillar with a concave air side and a convex mold side. Using higher solids content sols and slower drying processes results in reduced cupping due to drying shrinkage. The materials and process parameters are optimized to compensate for the differential shrinkage as well as to keep the pillars flat. Optimal conditions for producing sol-gel pillar bodies may produce discrete pillars that are suitable for use in vacuum insulated glazing without further modification.
  • a modified sol-gel process involving densification of an aerogel intermediate has been shown to greatly improve fidelity and minimize cupping or distortion during the drying process.
  • a modifying additive by an impregnation process.
  • a water-soluble salt can be introduced by impregnation into the pores of the calcined, pillar bodies. Then the pillar bodies are prefired again. This option is further described in European Patent Application Publication No. 293,163.
  • the pillar bodies were calcined at approximately 650 degrees Celsius and then saturated with a mixed nitrate solution of the following concentration (reported as oxides): 1.8% each of MgO, Y2O3, Nd 2 0 3 and La 2 0 3 .
  • the excess nitrate solution was removed and the saturated pillar bodies with openings were allowed to dry after which the pillar bodies were again calcined at 650 degrees Celsius and sintered at approximately 1400 degrees Celsius. Both the calcining and sintering was performed using rotary tube kilns.
  • a method of making a pillar body includes (a) providing a mold having a mold cavity, wherein the mold cavity includes the inverse shape corresponding to at least one of a chamfered peripheral edge and a rounded peripheral edge (b) positioning a reaction mixture within the mold cavity, (c) polymerizing the reaction mixture to form a shaped gel body that is in contact with the mold cavity, (d) removing the shaped gel body from the mold cavity, wherein the shaped gel body retains a size and shape identical to the mold cavity, (e) forming a dried shaped gel body by removing the solvent medium, (f) heating the dried shaped gel body to form a sintered body.
  • the sintered body has a shape identical to the mold cavity including at least one of a chamfered peripheral edge and a rounded peripheral edge but may be reduced in size proportional to an amount of shrinkage.
  • the reaction mixture may be as described above.
  • the dimensions of the mold cavity may be adjusted to account for the shrinkage.
  • the pillar body may be a polymer composite, including a binder, i.e. a polymer binder.
  • the binder may be based on thermally stable organic, inorganic, or hybrid polymers. These materials are typically dimensionally stable upon exposures to temperatures up to 350 °C.
  • the binder material has a low thermal conductivity, which would reduce the transfer of heat from the exterior through to the interior window pane.
  • Thermally stable binders include, but are not limited to, at least one of: polyimide, polyamide, polyphenylene, polyphenylene oxide, polyaramide (e.g., the KEVLAR product from Dupont), polysulfone, polysulfide, polybenzimidazoles, and polycarbonate.
  • polyimide polyamide
  • polyphenylene polyphenylene oxide
  • polyaramide e.g., the KEVLAR product from Dupont
  • polysulfone polysulfide
  • polybenzimidazoles polycarbonate
  • One exemplary binder that may be used is the ULTEM product (polyetherimide) manufactured by SABIC Innovative Plastics.
  • Another exemplary binder is an imide-extended
  • the polymer binder may include thermally stable inorganic, siloxane, or hybrid polymeric species. These materials are typically dimensionally stable upon exposures to temperatures up to 350 °C.
  • Amorphous organopolysiloxane networks a chemical bond network derived from condensation of organosiloxane precursors, is an example of a suitable thermally stable polymeric binder.
  • Silsesquioxanes or polysilsesquioxanes are derived from fundamental molecular units that have silicon coordinated with three bridging oxygen atoms. Because of this, silsesquoxanes can form a wide variety of complex three-dimensional shapes.
  • polysilsesquioxanes can be used, for example, polymethylsilsesquioxane, polyoctylsilsesquioxane, polyphenylsilsesquioxane and polyvinylsilsesquioxane.
  • Suitable specific polysilsesquioxanes include, but are not limited to, acrylopoly oligomeric silsesquioxane (Catalog # MA0736) from Hybrid Plastics of Hattiesburg, Mississippi; polymethylsilsesquioxane from Techneglas of Columbus, Ohio and sold under the label GR653L, GR654L, and GR650F; polyphenylsilsesquioxane from Techneglas of Columbus, Ohio and sold under the label GR950F; and
  • the polymer binder may also comprise other alkoxysilanes, such as
  • R may be an alkyl, alkylaryl, arylalkyl, aryl, alcohol, polyglycol, or polyether group, or a combination or mixture thereof;
  • the one or more alkoxysilanes including mono-, di-, tri-, and tetraalkoxysilanes may be added to control the crosslink density of the organosiloxane network and control the physical properties of the organosiloxane network including flexibility and adhesion promotion.
  • alkoxysilanes include, but are not limited to,
  • Such ingredients may be present in an amount of about 0 to 50 weight percent.
  • the polymer composite includes nanoparticles.
  • the nanoparticles may include silica, zirconia, titania, alumina, clay, metals, or other inorganic materials.
  • the loading of the nanoparticles is typically greater than 50 vol%.
  • the body may further include a functional layer on at least a portion of the body.
  • Functional layers or coating may be added as a layer or an enveloping coating around a pillar body.
  • Functional coatings have been disclosed in pending U.S. Appl. No. 14/025958, titled "VACUUM GLAZING PILL ARS FOR
  • the functional layer may include at least one of a compliant layer comprising a thermally stable polymer, a compliant layer comprising inorganic nanoparticles, a ferromagnetic layer, an electrically conductive layer, a statically dissipative layer and an adhesive; and optionally, wherein the adhesive comprises a sacrificial material.
  • a compliant planarization layer is one example of a functional layer that may be coated as a layer or an enveloping coating around a pillar body, e.g. a sintered ceramic pillar body, and is a thermally stable crosslinked nanocomposite that serves to flatten and smooth one or both of the major pillar body surfaces.
  • the planarization layer may also allow for a slight compression of the pillar during the fabrication of an insulated glass unit and thus reduce the likelihood of glass crack initiation or propagation upon evacuation to reduced pressure or to other environmental impacts.
  • the planarization layer comprises an organic, inorganic, or hybrid polymeric binder and an optional inorganic nanoparticle filler
  • the polymeric binder may include thermally stable organic polymeric species. These materials are typically dimensionally stable upon exposures to temperatures up to 350 °C.
  • the binder material has a low thermal conductivity, which would reduce the transfer of heat from the exterior through to the interior window pane.
  • Thermally stable organic polymeric component may be selected from thermally stable binders, thermally stable inorganic, siloxane, or hybrid polymeric species previously described.
  • a planarizing process for composite pillars can be carried out by thermal or radiation curing of the planarization material on one or both major surfaces of a pillar body while it is between two flat surfaces.
  • the composition may be identical to that of the composite pillars.
  • the planarization layer can have either adhesive or lubricant characteristic.
  • the compliant adhesive layer comprises a thermal or radiation sensitive silsesquioxane, a photoinitiator, and a nanoparticle filler.
  • the material can be crosslinked photochemically and then heated to initiate condensation of the silanol groups of the silsesquioxane, forming a durable, thermally stable material.
  • the adhesive layer can be used to set the final pillar height and define (minimize) the pillar height variation.
  • the orientation layer is a material applied to a pillar body while it is still in the mold.
  • the orientation can be on the mold side or the air side.
  • the air side is the exposed surface of the pillar when it is in the mold.
  • the function of the orientation layer is to physically or chemically differentiate the mold and air sides during placement of the pillars on a surface.
  • the orientation layer can be electrically conductive or statically dissipative, ferromagnetic, ionic, hydrophobic, or hydrophilic.
  • the frit glass coating is a dispersion of low melting glass microparticles in a sacrificial binder that is applied uniformly to the exterior of the pillar body.
  • a sacrificial binder is thermally decomposed and the frit glass flows to form an adhesive bond to one or both of the glass panes.
  • Sacrificial polymers such as, for example, nitrocellulose, ethyl cellulose, alkylene polycarbonates, [methjacrylates, and polynorbonenes can be used as binders.
  • the low COF layer may be a thermally stable material that promotes slip between the pillar body and a flat surface (e.g., one of the inner glass surfaces in a vacuum insulated glass unit).
  • the layer may comprise a monolayer of fluorosilanes, a fluorinated nanoparticle filled polyimide (e.g., Corin XLS, NeXolve, Huntsville, AL), a thin coating of a low surface energy polymer (e.g., PVDF or PTFE), a diamond-like carbon (DLC) layer, or a lamellar layer comprising graphite, or other thermally stable lubricant materials.
  • a fluorosilanes e.g., Corin XLS, NeXolve, Huntsville, AL
  • a thin coating of a low surface energy polymer e.g., PVDF or PTFE
  • DLC diamond-like carbon
  • the present disclosure includes a vacuum insulated glass unit having pillars, comprising: a first glass pane; a second glass pane opposite and substantially co-extensive with the first glass pane; an edge seal between the first and second glass panes with a substantial vacuum gap between the first and second glass panes; and a plurality of pillars, according to any one of the previously described pillar embodiments of the present disclosure, disposed between the first and second glass panes.
  • the use of pillars in IGUs is known in the arts and the pillars of the present disclosure can be included in an IGU using conventional techniques.
  • a vacuum insulated glass unit 400 is shown in FIGS. 8A and 8B.
  • Unit 400 includes two panes of glass 411 and 412 separated by a vacuum gap. Pillars 414 in the gap maintain the separation of glass panes 411 and 412, which are hermetically sealed together by an edge seal 413, which may be a low melting point glass frit.
  • Vacuum glazing pillar articles were prepared by using sol casting and molding methods with organic burnout and sintering processes.
  • the resultant constructions as shown in the following examples, provide pillars with reduced surface area that allow evacuation of air from the pillar interior and prevent interlacing of the pillars during bulk processing.
  • Sol compositions are reported in mole percent inorganic oxide.
  • the following hydrothermal reactor was used for preparing the Sol.
  • the hydrothermal reactor was prepared from 15 meters of stainless steel braided smooth tube hose (0.64 cm inside diameter, 0.17 cm thick wall; obtained under the trade designation "DUPONT T62 CHEMFLUOR PTFE” from Saint-Gobain Performance Plastics, Beaverton, MI). This tube was immersed in a bath of peanut oil heated to the desired temperature.
  • a precursor solution was prepared by combining the zirconium acetate solution (6,200 grams) with DI water (2074.26 grams). Yttrium acetate (992.62 grams) were added while mixing until fully dissolved. The solids content of the resulting solution was measured gravimetrically (120°C/hr. forced air oven) to be 22.30 wt. %. D.I. water (2,289 grams) was added to adjust the final concentration to 19 wt. %. The resulting solution was pumped at a rate of 11.48 ml/min. through the hydrothermal reactor. The temperature was 225°C and the average residence time was 42 minutes. A clear and stable zirconia sol was obtained.
  • the resulting sol was concentrated (35- 45 wt. % solids) via ultrafiltration and further diafiltered using a membrane cartridge (obtained under the trade designation
  • M21 S-100-01P from Spectrum Laboratories Inc., Collinso Dominguez, CA).
  • the final sol composition was 34.68 wt. % oxide and 3.70 wt.% acetic acid.
  • a polypropylene tool was generated from the master tool.
  • a 0.0625 inch thick (0.159 cm) sheet of polypropylene (available from McMaster Carr, Elmhurst, IL, USA) was placed on top of the master tool and embossed for 20 minutes at 383°F (195°C) and 6 psi using a stainless steel platen and the appropriate amount of weight to generate 6 psi pressure. The pressure was released by removing the weights and temperature was reduced to 75°F (24°C) and the polypropylene polymer tool was separated from the master tool. Then, the polypropylene tool was annealed between 2 glass plates at 248°F (120°C) for 20 mins.
  • Example 1 Micro-molded, structured, C-shaped pillars
  • a precursor solution was prepared and processed similar to the sol batch preparation procedure described above except that the composition of the sol was Zr0 2 (97.7 mol %) /Y2O3 (2.3 mol %) Sol.
  • the sol composition after processing via one or more of ultrafiltration, diafiltration and distillation was 40.84 wt. % oxide and 4.00 wt.% acetic acid.
  • the concentrated sol (437.40 grams) was charged to ajar and combined with diethylene glycol monoethyl ether (26.32 grams), MEEAA (4.68 grams), acrylic acid (27.03 grams), isobornyl acrylate (“SR506”) (24.64 grams), 1,6-hexanediol diacrylate (“SR238”) (10.11 grams), and a hexafunctional urethane acrylate ("CN975") (18.23 grams).
  • IRGACURE 819 (2.34 grams) was dissolved in ethanol (86.98 grams) and charged to the sol. The sol was passed through a 1 micron filter.
  • Casting Sol2 was cast into a polypropylene tool containing structured, C-shaped structures with dimension of about 1000 microns across by 400 microns deep.
  • the mold was adhered to a 2" x 3" (5 cm x 7.5 cm) glass plate with doubled sided tape.
  • the sol was flood coated onto the tool using a pipette.
  • a PET film was then carefully placed over the filled tool to prevent significant void formation.
  • a 2" x 3" (5 cm x 7.5 cm) glass plate was then placed on top of the PET, pressure was applied by hand to remove excess sol and the construction was clamped together.
  • the sol was cured for 2 minutes using a 380 - 401 nm LED light source at 100% power (CF2000 rev. 3.0 available from Clearstone
  • the cured parts were removed from the tool by removing the clamps, the top glass plate and the PET film and applying a 0.5 inch (1.27 mm) diameter tip of an ultrasonic horn (Sonifer Cell disrupter, available from Branson Ultrasonics, Danbury, CT, USA) to the backside of the polypropylene tool with the equipment set at continuous and the output set at 5 on the analog dial.
  • the parts were allowed to drop onto a nylon mesh screen. This allowed the C shaped pillars to dry equally from all sides at room temperature for up to 24 hours.
  • the dried C shaped xerogels were then burned out and sintered as follows:
  • the dried pillars are placed in an alumina crucible, then heated in air according to the following schedule:
  • a C-shaped pillar of Example 1 is shown in the SEM images of FIG. 9A (top view) and FIG. 9B (perspective view).
  • the C-shaped pillar of Example 1 had a segment angle theta of about 300 degrees. Pillars of similar design as that of Example 1 having segment angle theta of about 330 degrees (similar to FIGS. 3 A and 3B) and theta of about 240 degrees (similar to FIGS 5A and 5B) were also prepared. Pillars having a segment angle theta of 240 degrees and 300 degrees were found to interlace during bulk processing and handling.
  • a pillar design having a segment angle theta of about 330 degrees did not interlace at all.
  • the pillars made in these examples had a plurality of first structures on the top surface only.
  • Example 2 Micro-molded, C-shaped pillars with structure on top and bottom surfaces
  • the sol (97.7 mol% Zr0 2 /2.3 mol% Y 2 Cb) was cast into a polypropylene tool containing structured, C shaped structures with dimension of about 1200 microns across by 400 microns deep.
  • the mold was adhered to a 2"x3" (5 x 7.5 cm) glass plate with doubled sided tape.
  • the sol was flood coated onto the tool using a pipette.
  • a 2"x3" (5 x 7.5 cm) glass plate was then placed on top of the structured PET film, pressure was applied by hand to remove excess sol and the construction was clamped together.
  • the sol was cured for 2 minutes using a 380 - 401 nm LED light source at 100% power (CF2000 rev. 3.0 available from Clearstone Technologies Hopkins, MN, USA).
  • the cured structured, C shaped parts were removed from the tool. This was done by removing the glass cover plate and structured film immediately followed by applying a 1 ⁇ 2 inch
  • the dried pillars are placed in an alumina crucible, then heated in air according to the following schedule:
  • Example 2 The resulting C-shaped pillars of Example 2 had a segment angle theta of about 300 degrees and had structure on both surfaces. These pillars interlaced during bulk processing and handling and were challenging to unlace.

Landscapes

  • Engineering & Computer Science (AREA)
  • Civil Engineering (AREA)
  • Structural Engineering (AREA)
  • Joining Of Glass To Other Materials (AREA)

Abstract

La présente invention concerne des espaceurs servant à la fabrication de vitrage isolant, en particulier de vitrage isolant sous vide. L'invention concerne en outre un vitrage isolant comportant ces espaceurs. La présente invention concerne par ailleurs un espaceur destiné à être utilisé dans un vitrage isolant sous vide, l'espaceur comprenant un corps en forme de C ayant une épaisseur, une première surface de contact présentant une première superficie, une seconde surface de contact opposée présentant une seconde superficie et au moins une paroi latérale. La première surface de contact comprend au moins une première structure faisant partie intégrante de la première surface de contact, l'au moins une première structure ayant une première base de structure et une première face de structure opposée à la base, une épaisseur et une première superficie de face de structure.
PCT/US2017/018782 2016-03-07 2017-02-22 Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant WO2017155687A1 (fr)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US201662304709P 2016-03-07 2016-03-07
US62/304,709 2016-03-07
US201762451946P 2017-01-30 2017-01-30
US62/451,946 2017-01-30

Publications (1)

Publication Number Publication Date
WO2017155687A1 true WO2017155687A1 (fr) 2017-09-14

Family

ID=58192420

Family Applications (1)

Application Number Title Priority Date Filing Date
PCT/US2017/018782 WO2017155687A1 (fr) 2016-03-07 2017-02-22 Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant

Country Status (1)

Country Link
WO (1) WO2017155687A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220127901A1 (en) * 2019-02-08 2022-04-28 Nippon Sheet Glass Company, Limited Glass unit

Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0293163A2 (fr) 1987-05-27 1988-11-30 Minnesota Mining And Manufacturing Company Particules abrasives formées par imprégnation des céramiques, leur méthode de préparation et les produits obtenus
EP1004552A1 (fr) * 1998-05-01 2000-05-31 Nippon Sheet Glass Co., Ltd. Panneau de verre, procede de fabrication et espaceur pour ce panneau de verre
US6479112B1 (en) 1998-05-07 2002-11-12 Nippon Sheet Glass Co., Ltd. Glass panel and method of manufacturing thereof and spacers used for glass panel
US20040068023A1 (en) 2002-10-02 2004-04-08 3M Innovative Properties Company Multi-photon reactive compositons with inorganic particles and method for fabricating structures
US20090099537A1 (en) 2006-03-24 2009-04-16 Devoe Robert J Process for making microneedles, microneedle arrays, masters, and replication tools
US20100260950A1 (en) 2009-04-10 2010-10-14 Beijing Synergy Vacuum Glazing Technology Co., Ltd. Pillar arranged in vacuum glazing
US20120012557A1 (en) 2008-12-30 2012-01-19 David Moses M Method for making nanostructured surfaces
US20150233174A1 (en) * 2014-02-14 2015-08-20 Eversealed Windows, Inc. Method and apparatus for spacers for inter-pane cavity of vacuum insulating glass units and vacuum insulating glass units incorporating same
US20150293272A1 (en) 2012-11-21 2015-10-15 3M Innovative Properties Company Optical diffusing films and methods of making same
US20150306363A1 (en) 2012-12-27 2015-10-29 3M Innovative Properties Company Article with hollow microneedles and method of making

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0293163A2 (fr) 1987-05-27 1988-11-30 Minnesota Mining And Manufacturing Company Particules abrasives formées par imprégnation des céramiques, leur méthode de préparation et les produits obtenus
EP1004552A1 (fr) * 1998-05-01 2000-05-31 Nippon Sheet Glass Co., Ltd. Panneau de verre, procede de fabrication et espaceur pour ce panneau de verre
US6479112B1 (en) 1998-05-07 2002-11-12 Nippon Sheet Glass Co., Ltd. Glass panel and method of manufacturing thereof and spacers used for glass panel
US20040068023A1 (en) 2002-10-02 2004-04-08 3M Innovative Properties Company Multi-photon reactive compositons with inorganic particles and method for fabricating structures
US20070264501A1 (en) 2002-10-02 2007-11-15 3M Innovative Properties Company Multi-photon reactive compositions with inorganic particles and method for fabricating structures
US20090099537A1 (en) 2006-03-24 2009-04-16 Devoe Robert J Process for making microneedles, microneedle arrays, masters, and replication tools
US20120012557A1 (en) 2008-12-30 2012-01-19 David Moses M Method for making nanostructured surfaces
US20100260950A1 (en) 2009-04-10 2010-10-14 Beijing Synergy Vacuum Glazing Technology Co., Ltd. Pillar arranged in vacuum glazing
US20150293272A1 (en) 2012-11-21 2015-10-15 3M Innovative Properties Company Optical diffusing films and methods of making same
US20150306363A1 (en) 2012-12-27 2015-10-29 3M Innovative Properties Company Article with hollow microneedles and method of making
US20150233174A1 (en) * 2014-02-14 2015-08-20 Eversealed Windows, Inc. Method and apparatus for spacers for inter-pane cavity of vacuum insulating glass units and vacuum insulating glass units incorporating same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20220127901A1 (en) * 2019-02-08 2022-04-28 Nippon Sheet Glass Company, Limited Glass unit

Similar Documents

Publication Publication Date Title
US10550627B2 (en) Vacuum glazing pillars for insulated glass units and insulated glass units therefrom
US9878954B2 (en) Vacuum glazing pillars for insulated glass units
US20180066469A1 (en) Vacuum glazing pillars for insulated glass units and insulated glass units therefrom
US10988979B2 (en) Microoptics for glazing
JP5261817B2 (ja) 表面に微細凹凸パターンを有したセラミックス焼成体及びその製造方法
WO2017155687A1 (fr) Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant
JP6588913B2 (ja) 金属酸化物粒子
WO2017155779A1 (fr) Espaceurs de vitrage sous vide pour vitrage isolant et vitrage isolant les comportant
US20200002237A1 (en) Porous ceramic particle and porous ceramic structure
US20190152862A1 (en) Porous ceramic particle and porous ceramic structure
US11572315B2 (en) Thermal insulation member
JP2011176101A (ja) 電磁波吸収体及びその製造方法
WO2006097875A1 (fr) Methode de production d'un composant dote d'une structure de surface, composant ceramique, et application d'une telle methode
JP2020140173A (ja) 反射防止膜付きシリカ焼結体及びその製造方法

Legal Events

Date Code Title Description
NENP Non-entry into the national phase

Ref country code: DE

121 Ep: the epo has been informed by wipo that ep was designated in this application

Ref document number: 17708411

Country of ref document: EP

Kind code of ref document: A1

122 Ep: pct application non-entry in european phase

Ref document number: 17708411

Country of ref document: EP

Kind code of ref document: A1