EP2798399A1

EP2798399A1 - Multiple glazing with variable diffusion by liquid crystals and method of manufacture thereof

Info

Publication number: EP2798399A1
Application number: EP12824701.2A
Authority: EP
Inventors: Jingwei Zhang; Patrick Gayout
Original assignee: Saint Gobain Glass France SAS; Compagnie de Saint Gobain SA
Current assignee: Saint Gobain Glass France SAS; Compagnie de Saint Gobain SA
Priority date: 2011-12-29
Filing date: 2012-12-27
Publication date: 2014-11-05
Also published as: CA2861730C; US20140375915A1; CA2861730A1; MX369476B; US9891454B2; MX2014007907A; FR2985327B1; FR2985327A1; WO2013098527A1; CN104106000A; JP2015503774A; KR20140108315A

Abstract

The present invention provides multiple glazing with variable diffusion by liquid crystals (100), having first and second sheets of flat float glass (1, 2) held on the edge of their internal faces (11, 21) by a seal (7), in particular made of a given seal material, in particular substantially organic, first and second electrodes (3, 4), a layer (5) of liquid crystals of average thickness E between 5 and 15 μm including 5 μm and excluding 15 μm and incorporating spacers (6). The thickness of each of the first and second glass sheets is less than or equal to 6.5 mm and each of the coated internal faces of the first and second electrodes has a dioptric defect rating, expressed in millidiopters, of less than or equal to (I) where the thickness E of liquid crystals is in µm. The invention also relates to a method of manufacturing such glazing.

Description

VARIABLE DIFFUSION MULTIPLE GLAZING BY LIQUID CRYSTALS, ITS MANUFACTURING PROCESS

The invention relates to the field of electrically controllable glazings with variable optical properties and more particularly relates to a liquid crystal variable diffusion glazing, provided with a layer of liquid crystals between two glasses and reversibly alternating by application of an electric field. alternative between a transparent state and a non-transparent state.

Glazes are known whose characteristics can be modified under the effect of a suitable power supply, especially the transmission, absorption, reflection in certain wavelengths of electromagnetic radiation, especially in the visible and / or in the infrared, or the light diffusion.

The electrically controllable liquid crystal glazing can be used everywhere, in both the construction sector and the automotive sector, whenever the view through the glazing is to be prevented at given times.

WO9805998 discloses a liquid crystal multiple glazing unit comprising:

- two sheets of float glass ("float" in English) of 1 m ² and 6 mm thick sealed on the edge of their inner faces by an adhesive seal of epoxy resin,

two electrodes in electrically conductive layers based on Sn0 ₂ : F directly on the internal faces of the glasses,

- A liquid crystal layer based on PSCT ("Polymer Stabilized Cholesteric Texture" in English) of 15 μηη and incorporating spacers in the form of glass beads of 15 μηη, directly on the electrodes. The glasses are brought into contact by lowering the second glass with an inclined angle on the second glass to enclose the liquid crystal layer as shown in Figure 2 and described on page 8.

Then, after formation of the seal, the glasses are pressed by passing between two rollers to distribute the liquid crystal layer by evacuating trapped air as shown in Figure 3.

The optical performance and reliability of this glazing can be improved. In addition, such a glazing is expensive, heavy, bulky, especially difficult to handle.

An object of the invention is to develop a multiple crystal glazing reliable liquids, with satisfactory optical performance and preferably compact.

For this purpose, the present invention firstly proposes a multiple glazing with variable diffusion by liquid crystals, having:

first and second sheets of float plane glass held at the edges of their internal faces by a seal, in particular a given seal material, in particular essentially organic material,

on the inner faces of the first and second glass sheets, first and second electrodes in the form of transparent electrically conductive layers provided with power supply,

and, on the first and second electrodes, a layer containing liquid crystals in polymeric material (or polymer matrix), the liquid crystal layer reversibly alternating between a transparent state and a translucent state by application of an alternating electric field, layer of average thickness E between 5 and 15 μηη including 5 μηη and excluding 15 μηη; and preferably 8 μηη, better 10 μηη to 14 μηη, liquid crystal layer incorporating spacers, especially transparent.

Each of the first and second sheets of glass has a thickness less than or equal to 6.5 mm and each of the internal faces coated with the first and second electrodes has a dioptric defects rating, expressed in millidioptrie (or mdt), less than or equal to 2 + 2E, where the thickness E of liquid crystals is in μηι.

We can prefer a thickness E greater than or equal to 8 μηη and even 10 μηη to more easily guarantee the optical performance.

The Applicant has discovered the relationship between the quality of the glasses and the optical performance of multiple liquid crystal glazing with a particularly low liquid crystal thickness.

Of course, the thickness of the first glass sheet may be different from or equal to the thickness of the second glass sheet. The requirement on the rating of dioptric defects is valid for each.

FIG. 1 shows, as comparative glazing, an assembly of two standard thin glasses 10, 20, for example 1, 7 mm, facing each other, forming a space between them containing a layer of liquid crystals. thickness lowered to 12 μηι. the inner surfaces 11 ', 21' have flatness defects, the liquid crystal thickness is variable. In the "off" state (translucent state), the light transmission, closely related to the thickness of the liquid crystal layer, is therefore non-uniform. The quality of the product is therefore unacceptable, because of the dark and clear areas visually observable.

In order to guarantee good optical uniformity, the coated glasses must therefore have limited dioptric defects.

The glasses according to the invention ensure a sufficiently uniform thickness of the liquid crystal layer over the entire surface and therefore few variations in optical performance. This avoids a scrap rate of glazing and thus improves its reliability.

Here we define a dioptric defect and a measurement method.

The profile of the inner face of each glass sheet (coated or uncoated) in question can be described by y (x) where x denotes the position on the internal face. The variation of this profile can be characterized by the optical power in reflection POR which is defined by the following relation:

The variation of y (x) is due to the two phenomena:

- ripples of the glass sheet,

- thickness defects (non-parallelism of the 2 faces of the glass sheet).

This quantity is expressed in diopter (m ^"1 ) for y (x) expressed in meters.

If the second derivative y "(x) is zero, it means that the internal face of the glass is perfectly flat, if the second derivative is less than 0 it means that the inner face of the glass is concave of the glass and if the second derivative is greater at 0 it means that the inner face of the glass is convex.

The method for measuring the flatness y (x) of the internal face of the glass is a non-contact optical measurement method which consists of analyzing the contrast at any point of a so-called ombroscopic image obtained by reflection of a homogeneous light source on the inner surface of the glass.

The unmeasured outer face of the glass sheet is wetted with a liquid of index close to that of the glass in order to eliminate any reflection of the light on this face and keep only the image of the directly illuminated inner face.

Flatness is thus measured every millimeter on the illuminated surface of the internal face. Each point is quantified by physical unit of optical power in millidioptrie (mdt = diopter / 1000), comparable to convergent and divergent lenses.

The final flatness is quantified by a rating of dioptric defects, which corresponds to the standard deviation of all measurements. This note, expressed in millidioptrie (mdt), perfectly characterizes the flatness of the measured surface. The note increases when the flatness deteriorates.

For a given rating of dioptric defects, the amplitude of the variation of y (x) also depends on the periodicity or pitch.

By way of example, for a sinusoidal y (x) profile with a pitch of 30 mm, a dioptric defect of 10 mdt corresponds to a profile variation of approximately +/- 0.20μη "ΐ. cases, the variation of space of an assembly of two sheets of glasses (thus variation of the thickness E of liquid crystals) is then doubled, of approximately +/- 0.40 μηη. 15 mm, the same dioptric defect of 10 mdt corresponds to a profile variation of +/- 0.05 μηι, and the variation of the thickness E of liquid crystals is therefore +/- 0.10 μηη in the worst case.

The dioptric flaw pitch of a float glass sheet covers a range of a few millimeters to a few tens of millimeters. Being closely related to the uniformity of the liquid crystal thickness E, the uniformity of light transmission in "off" state is the consequence of all the dioptric defects at all steps.

The uniformity of light transmission in "off" state is also conditioned by the average thickness E of CL. The lower the thickness E is, the less can be tolerated a variation in thickness. This is why according to the invention a note is established according to the average thickness.

The dioptric defects of float glass are mainly related to the speed of movement of the glass (taken from the line). The faster the glass scroll speed, the greater the dioptric defects. For a capacity (or tonnage, daily) and a given gross glass width, the speed of glass scroll is inversely proportional to the thickness of the glass sheet. Thus, the thinner the glass sheet, the higher the glass scroll speed and the greater the dioptric defects.

Thus, one can not use a thickness at random because it is the dioptric quality of the glass which determines the possible thickness of the glass. The invention allows us for example to use a thickness as small as possible while guaranteeing the optical quality of the final product. For example, one can choose 2 mm glasses provided that these glasses are produced with a firing sufficiently low to guarantee the limitation of dioptric defects.

For a 6 mm glass if the tonnage is too high for example 2000 tons / day dioptric defects are too important for this range of low liquid crystal thicknesses.

The glass of the first and / or second glass sheet may preferably have a light transmission T _L greater than or equal to 70%, preferably greater than or equal to 80% or even 90%. The glass is preferably transparent and colorless.

It may be a clear or extra-clear mineral glass. Clear glass typically contains a weight content of iron oxide in the range of 0.05 to 0.2%, while extra clear glass typically contains about 0.005 to 0.03% iron oxide.

The glass of the first and / or second glass sheet may, however, be dyed in the mass by appropriate dyes, for example blue, green, gray or bronze. It is generally preferred that the glass has a color in transmission as neutral as possible, especially in gray. It is particularly possible to use the range of tinted glasses marketed under the name PARSOL (bronze, green or gray) by the company SAINT-GOBAIN GLASS.

The glass, in particular stained glass, may preferably have a light transmission T _L greater than or equal to 10% - for example in a context where the medium on the side of the outer face (opposite to the face with the electrode) is very bright - and preferably is greater than or equal to 40%.

Float glass is obtained in a known manner by a process of pouring the molten glass on a bath of molten tin ("float" bath). In this case, the electrode can be deposited on the "tin" face as well as on the face

"Atmosphere" of the glass. By "atmosphere" and "tin" faces are meant the faces having respectively been in contact with the atmosphere prevailing in the float bath and in contact with the molten tin. The tin side contains a small surface amount of tin that has diffused into the glass structure.

The electrode layer (s) has no significant influence on dioptric defects.

Also if a "naked" float glass is suitable, the glass coated with an electrode layer will also be suitable.

The electrode layer (s) is for example:

a stack of layers comprising at least one (thin) layer of silver between two (thin) dielectric layers (non-dielectric dielectric) metallic, typically oxide or metal nitride),

a transparent conductive oxide layer called TCO.

The TCO layer is preferably a layer of tin oxide and indium (ITO). Other layers are possible, among which are the following (thin) layers:

- based on indium zinc oxide (called "IZO"), indium gallium and zinc oxide (IGZO),

based on doped zinc oxide, preferably gallium or aluminum oxide (AZO, GZO), based on niobium-doped titanium oxide, based on cadmium stannate or zinc,

- based on fluorine-doped tin oxide (SnO ₂ : F), based on tin oxide doped with antimony.

We can also add:

one or more dielectric sublayers (dielectric in the non-metallic sense, typically oxide or metal nitride) under the TCO layer (underlayer directly on the glass),

and / or one or more dielectric overcoats (dielectric in the non-metallic sense, typically oxide or metal nitride) on the TCO layer (overlayer in contact with the liquid crystal layer).

An underlayer or an overlayer is for example a thin layer (typically less than 150 nm).

The electrode in layer (s) (in particular a stack of thin layers, in particular with underlayer (s) and / or overlayer (s)) is preferably deposited by vacuum deposition (physical vapor deposition "PVD", chemical vapor deposition "CVD" etc.). Deposition by sputtering (magnetron) is preferred.

The electrode layer (s) (including a stack of thin layers, in particular with underlayer (s) and / or overlayer (s)) therefore has no significant influence on dioptric defects. Also if a "naked" float glass is suitable, float glass coated with such layers will also be suitable. Of course, for the sake of simplicity and economy, it is preferred to select suitable float glasses rather than having to smooth (polish, etc.) any glass obtained by another manufacturing process.

The invention also makes it possible to produce multiple liquid crystal glazings with a width greater than 1 m.

In a preferred embodiment,

for a thickness E less than 8 μηη, one or even each of the first and second sheets of glass has a thickness of between 4.5 mm and and 5.5mm including these values, in particular 4 ± 0.2μη "ΐ, 5 ± 0.2μηΊ which are conventional thicknesses,

or

for a thickness E greater than or equal to 8 m (and always less than 15 μm), one or even each of the first and second sheets has a thickness between 2.5 mm and 5.5 mm including these values, in particular 3 ± 0.2μη "ΐ, 4 ± 0.2μηΊ and 5 ± 0.2μη" ΐ, in particular by production on a Float line with a capacity of at least 550 tonnes / day and preferably limited to 900 tonnes / day.

Furthermore, the seal is of given width L and can preferably be interrupted in its width by one or more vents defining each of the lateral ends of the seal, and for each vent an additional material forms a bridge between the lateral ends of the seal, in particular in said joint material thus forming continuity of material.

In the multiple glazing liquid crystal of the prior art, the seal serving for sealing is continuous.

With one or more vents - supplemented by an additional material - interrupting according to the invention the joint of such a multiple liquid crystal glazing, the optical performance (in the off state) is improved, notably by participating in the edge zones. the liquid crystal layer to uniformly distribute the liquid crystal layer.

A liquid crystal variable liquid crystal multiple multiple glazing having:

first and second flat glass sheets held at the edges of their internal faces by a joint, in particular a given joint material, with one or more vents, supplemented by an additional material;

and on the first and second electrodes, a layer containing liquid crystals in polymeric material, the liquid crystal layer reversibly alternating between a transparent state and a translucent state by application of an alternating electric field, average thickness E between 5 and 15 μηη or even 15 to 60 μηη,

constitutes an invention in itself.

However, in a preferred embodiment, it is coupled to the glazing multiple liquid crystal with the thin liquid crystal layer as defined above and with the glasses as defined above each having a limited diopter note.

Furthermore, all the liquid crystal systems known as "NCAP" (Nematic Curvilinearly Aligned Phases) or "PDLC" (Polymer Dispersed Liquid Crystal) or "CLC" (Cholesteric Liquid Crystal) can be used. ) or NPD-LCD (Non-Homogeneous Polymer Dispersed Liquid Crystal Display).

These may further contain dichroic dyes, especially in solution in the liquid crystal droplets. It is then possible to modulate the light scattering and the light absorption of the systems.

It is also possible to use, for example, cholesteric liquid crystal-based gels containing a small amount of crosslinked polymer, such as those described in patent WO-92/19695. More broadly, one can choose "PSCT" (Polymer Stabilized Cholesteric Texture in English).

It is possible to use multistable liquid crystals and in particular it is possible to use bistable smectic liquid crystals, for example as detailed in patent EP2256545, which switch under the application of an alternating electric field in pulsed form and which remain in the switched state until the application of a new pulse.

Naturally, the liquid crystal system may extend substantially over the entire surface of the glazing (excluding outgassing), or on (at least) a restricted area. The liquid crystal system may be discontinuous, in several pieces (for example of the pixel type).

It is possible to use liquid crystal variable diffusion multiple glazing as previously defined as glazing in vehicles or buildings.

The glazing according to the invention can be used in particular:

- as an internal partition (between two rooms or in a space) in a building, in a means of locomotion terrestrial, aerial, aquatic (between two compartments, in a taxi etc),

- as glazed door, window, ceiling, tiling (floor, ceiling),

- as vehicle rearview mirror, side glazing, roof of a means of locomotion on land, air, water,

- as a projection screen,

- as a shop facade, showcase including a counter. Naturally, the glazing according to the invention can form all or part of a partition and other window (type transom etc.).

By lowering the thickness of the layer (and therefore the amount of encapsulated active mixture) below 15 μηι, the cost of material is reduced.

Moreover, the spacers may preferably be made of a transparent plastic material. The spacers determine (roughly) the thickness of the liquid crystal layer. For example, polymethylmethacrylate (PMMA) spacers are preferred.

The spacers are preferably in terms of optical index (substantially) equal to the optical index of (the matrix of) the liquid crystal layer.

The spacers are for example in the form of beads.

The subject of the invention is also a process for producing a liquid crystal variable diffusion multiple glazing unit as defined above and comprising the following steps:

the formation of the seal comprising the application of the seal material (preferably essentially organic, in particular epoxy resin) to the first float glass sheet (at the edge) provided with the first electrode,

- (before or after the formation of the seal), the liquid deposition of the liquid crystal layer of an average thickness E on the first float glass sheet provided with the first electrode and optionally on the second float glass sheet equipped with the second electrode,

after the formation of the seal and the deposition of the liquid crystal layer, bringing the first and second glass sheets into contact, in particular by calendering or pressing,

and before contacting the first and second glass sheets, the formation of said gasket outlet (s) each defining the lateral ends of the gasket, by the discontinuous application of the gasket material and / or by the continuous application of the joint material and the creation of interruptions forming the vents.

Preferably, at least two vents are positioned facing a first sheet edge (straight or curved sheet) and preferably at least two other vents facing a second edge opposite the first edge, these edges corresponding to the edges of the calendering direction, in case of calendering.

In the case of pressing, in particular, at least two vents are positioned next to a third edge of the sheet adjacent to the first edge (and to the second edge) and to the minus two other vents next to a fourth edge opposite the third edge.

The method may further comprise the application of the additional material, forming a bridge between the lateral ends of the seal.

The additional material may be of said seal material thus forming continuity of material, preferably essentially organic, especially epoxy resin.

Preferably the width between the lateral ends of the seal may be at least 5 mm, for example 10 mm.

Other details and characteristics of the invention will appear from the detailed description which follows, made with reference to the appended drawings in which:

FIG. 1 (already described) represents a schematic sectional view of a reference liquid crystal variable diffusion multiple glazing, not in accordance with the invention,

FIG. 2 represents a schematic cross-sectional view of a variable-liquid crystal variable diffusion multiple glazing of a small thickness in a first embodiment according to the invention,

FIG. 3 shows the circuit diagram of the measurement of the dioptric fault score,

FIG. 4 shows the principle of forming an ombroscopic image on a screen from a flatness profile of the glass Y (x),

FIG. 5 shows an example of local illumination profile E (x) and average illumination E0 (x),

FIG. 6 represents a schematic top view of a variable-liquid crystal variable-diffusion glazing unit according to the invention showing in particular the seal and the vents,

FIG. 6bis shows a schematic top view of the multiple liquid crystal variable diffusion glazing, showing in particular and the seal and the vents, in a variant of FIG.

- Figure 7 shows a schematic top view of the manufacture of multiple glazing liquid crystal variable diffusion according to the invention showing in particular the seal and the vents.

The exemplary embodiment shown in FIG. 2 shows the design of the multiple liquid crystal glazing according to the invention in a first embodiment.

On two sheets of float glass 1 and 1 'are disposed on the inner faces 1 1, 21 an electrically conductive layer 3, 4 with a thickness of about 20 to 400 nm, external surface 21, 31 made of indium oxide and tin (ITO) for example. ITO layers have a surface electrical resistance of between 5 Ω / Ώ and 300 Ω / Ώ. Instead of the layers made of ITO, it is also possible to use for the same purpose other layers of electrically conductive oxide or silver layers whose surface resistance is comparable.

The layer 5 of liquid crystals, which may have a thickness of about 5 to 15 μηη (excluded), is located between the electrode layers 3 and 4. The thickness is preferably at least 8 μηη and even 10 μηη (about).

The liquid crystal layer 5 contains spherical spacers. The spacers 6 consist of a transparent polymer.

In order to ensure the uniformity of the thickness E of the liquid crystal layer and thus ensuring the optical performance of the liquid crystal glazing, glasses 1, 1 'are chosen with their electrodes 3, 4 each with a dioptric defects score that complies with to the invention, note measured by ombroscopy in reflection.

The basic principle is related to geometrical optics. The diagram of the assembly is shown in FIG.

A light flux is projected from a thin source, such as a projector 100, onto the face of the glass sheet 11 (coated or not with the electrode) intended to be the internal face. On a screen 300 is observed an image projected after reflection on the inner face 1 1 of the glass sheet. This image is captured by a digital camera 200 to be processed. The reflection on the second face 12 is neutralized through the use of a wet black fabric placed behind the glass 1 and on which is sticking the glass by capillarity.

FIG. 4 gives the principle of forming an ombroscopic image on the screen 300 from a flatness profile of the glass Y (x). A concave zone on the glass

(Convergent defect) causes a concentration of the reflected incident light 1 10 and thus a local over-illumination on the screen 300. A convex zone on the glass (divergent defect) causes a spreading of the reflected incident light 120 and therefore a sub - local illumination on the screen 300.

FIG. 5 shows an example of local illumination profile E (x) and average illumination E0 (x).

When the local illumination E (x) is equal to the average illumination E0 (x), the contrast is zero, and consequently Y "(x) = 0 and the optical power is zero. When the local illumination E (x) is greater than the average illumination E0 (x) the contrast is negative and Y "(x) <0. It is then a convergent defect, which corresponds to a concavity on glass.

When the local illumination E (x) is lower than the average illumination E0 (x) the contrast is positive and Y "(x)> 0. It is then a divergent defect which corresponds to a convexity on glass.

Knowing that the variations of flatness are more important in the direction of the net width, to explain the principle of operation of the apparatus we will consider a profile of flatness in the plane perpendicular to the direction of casting and perpendicular to the surface of the glass.

It can be shown from the laws of geometrical optics and the conservation of energy that there is a relation between the illuminance measured on the screen E (x) corresponding to a point of abscissa x on the glass and the Y (x) profile of the glass surface.

Some geometrical simplifications are made from the following elements: the assembly is in quasi-normal reflection and the source is considered punctual, we have the following relation: With:

Y (x): glass profile

D: the distance between glass and screen

E ₀ : average illumination in x (that which one would have without flatness)

That is the optical power in reflection POR (in diopter): dx ² D with the contrast C (x) such that

E ₀ - E (x)

E (x) The contrast corresponds to the visual perception of the "lineage" (here dashed since we consider a profile and not a surface) found on the ombroscopic image projected on the screen. A processing software calculates for each pixel of the image, the contrast and therefore the optical power in reflection POR.

The dioptric fault score (in millidioptria) reflects the homogeneity of the optical powers and is in fact the standard deviation σ of the distribution of the optical powers in reflection on the int face. with

(POr ² ) _ij : Average over the entire inner face, of the square of the optical powers : Square over the entire internal face of the average optical power The rating must be less than or equal to 2 + to ensure optical quality in sufficient transmission, that is to say a good homogeneity of the light transmission in "off" state ".

For a liquid crystal thickness of 12 μηι, a score of less than 10 is required.

For a liquid crystal thickness of 10 μηι, a score of less than 8.7 is required.

For a thickness of liquid crystals, 8 μηη requires a score lower than equal to 7.3.

By way of example, for a Float line with a capacity of 600 tonnes / day with a gross glass width of 3.5 m:

- the 2.1 mm glass rating is less than 22 mt,

- the note of the glass of 3 mm is less than 1 1 mdt,

- the note of the glass of 4 mm is less than 8 mdt approximately,

- the note of the glass of 6 mm is less than or equal to 5 mdt approximately.

Furthermore, for the liquid crystal layer, it is also possible to use known compounds, for example the compounds described in document US Pat. No. 5,691,795. The liquid crystal compound of Merck Co., Ltd, sold under the trade name "Cyanobiphenyl" Nematic Liquid Crystal E-31 LV "also proved to be particularly suitable. In the case of this embodiment, this product is mixed in a 10: 2 ratio with a chiral substance, for example 4-cyano-4 '- (2-methyl) butylbiphenyl, and this mixture is mixed in the ratio : 0.3 with a monomer, for example 4,4'-bisacryloylbiphenyl, and with a UV initiator, for example benzoin methyl ether. The mixture thus prepared is applied to one of the coated glass sheets. After curing the liquid crystal layer by irradiation with UV light, a polymer network is formed in which the liquid crystals are incorporated.

For the liquid crystal layer, PDLCs such as 4 - ((4-ethyl-2,6-difluorophenyl) -ethinyl) -4'-propylbiphenyl and 2-fluoro-4,4'-bis ( trans-4-propylcyclohexyl) biphenyl sold, for example, by Merck under the reference MDA-00-3506.

On the edge, the liquid crystal layer is sealed by an adhesive seal 5 which serves at the same time to connect the glass sheets 1, 1 'endowed with the electrodes firmly and permanently.

The seal adhesive material contains an epoxy resin.

As shown in FIG. 6, the seal 7 is of width L given and interrupted in its width by a plurality of vents 81 to 84 defining each of the joint lateral ends 71 to 74 '.

More specifically, the joint 7 is interrupted in its width by two vents 81 to 82 opposite a first edge of the glazing and by two other vents 83, 84 facing a second edge opposite the first edge, these edges corresponding to the edges of the assembly direction of the glasses, preferably by calendering.

For each vent an additional material 7 'forms a bridge between the adjacent lateral ends of the seal, in particular said seal material thus forming continuity of material as shown in Figure 6a.

At the initial stage ("off" state), that is to say before the application of a voltage, this liquid crystal glazing 100 is translucent, that is to say it transmits optically but n is not transparent. As soon as the current is connected, the liquid crystal layer passes under the action of the alternating electric field in the transparent state, that is to say the one in which the vision is not prevented.

The electrically controllable liquid crystal glazing is produced using a method described in detail hereinafter.

In an industrial continuous coating plant, using the reactive sputtering method supported by magnetic field, by float glass sheets according to the invention, are coated in successive spray chambers with a layer of ITO of an approximate thickness of 100 nm.

Two separate glass sheets of equal size and size desired are cut from a large sheet of glass coated in this manner and prepared for further processing.

The two separate glass sheets cut to the desired measurements first undergo a washing operation.

The liquid crystal layer mixed with the spacers is then applied to one of the two glass sheets thus treated.

As the two separate glass sheets are then permanently and tightly connected to each other at their edges by a seal, the edge portion of the glass sheet 1 is not coated to a width of about 2 to 10 mm.

The coating by the mass of liquid crystals is carried out by means of an operation called drip filling. For the application of the operation, a drip pouring apparatus is used which allows the deposition of drops of liquid crystals on a glass substrate, the poured amount being finely adjustable.

In another embodiment of the method, for printing the liquid crystal layer, a screen printing fabric of a mesh whose width is approximately 20 to 50 μηη and whose wire diameter is approximately 30 to 50 μηη.

The adhesive layer forming the gasket 7 is likewise applied directly along the edge of the glass sheet 24 before or after the deposition of the liquid crystal layer. It may have a width for example of 2 to 10 mm.

As shown in FIG. 7, provision is made for forming the plurality of a plurality of vents 81 to 84 of the size and distribution joint adapted to evacuate the excess liquid crystal layer, the vents 81 to 84 each defining two lateral ends. adjacent 71 to 74 'of joint 7.

Also, for this purpose, the application of the joint material is either discontinuous or is continuous and then followed by a creation of the vents (by removal of material 7).

Application of the additional material 7 'is then provided, forming a bridge between the lateral ends of the seal 71 to 74' preferably of said joint material, thus forming continuity of material.

When the two separate glass sheets are then pushed against each other, the adhesive layer 7 is compressed to the thickness E of the liquid crystal layer.

Vents 81 to 84 serve therefore:

- To evacuate the excess liquid crystal layer, and therefore to better control the layer thickness and thus to avoid loss of optical quality, - to degas the liquid crystal layer to avoid the subsequent formation of bubbles in the layer and thus again avoid a loss of optical quality. At least two vents are preferably positioned on the front edge of the calendering and at least two vents on the rear edge of the calendering.

The width of the lateral ends is an example of 10 mm. The more viscous liquid crystal layer, the more vents are used.

Then, we proceed to calendering or alternatively to pressing.

If the liquid crystal layer consists of a mixture of liquid crystals and a monomer, the polymerization operation is then carried out by irradiation with UV light.

Claims

Multiple liquid crystal variable diffusion (100) glazing, having:

first and second float plane glass sheets (1, 2) held at the edges of their inner faces (1 1, 21) by a seal (7), in particular of a given seal material,

on the inner faces of the first and second glass sheets, first and second electrodes (3, 4) in the form of transparent electrically conductive layers provided with power supply,

and, on the first and second electrodes, a layer (5) containing liquid crystals in polymeric material, the liquid crystal layer reversibly alternating between a transparent state and a translucent state by application of an alternating electric field. , liquid crystal layer (5) of average thickness E of between 5 and 15 μηη including 5 μηη and excluding 15 μηη, layer (5) of liquid crystal incorporating spacers (6), each of the first and second sheets of glass has a thickness less than or equal to 6.5 mm and each of the internal faces coated with the first and second electrodes have a dioptric defects rating, expressed in millidioptrie, less than or equal to ^ ⁺ ^ / ^ ^or layer thickness E liquid crystal is in μηι.

Multiple liquid crystal variable diffusion multiple glazing (100) according to claim 1, characterized in that

for a thickness E less than 8 μηη, one or even each of the first and second glass sheets (1, 2) has a thickness of between 4.5 mm and 5.5 mm including these values,

or

- For a thickness E greater than or equal to 8 μηι, one or even each of the first and second glass sheet (1, 2) has a thickness between 2.5 mm and 5.5 mm including these values.

Variable diffusion liquid crystal display (100) according to one of claims 1 or 2, characterized in that the seal (7) is of width L given and interrupted in its width by one or more vents (81 to 84) defining each of the lateral joint ends (71 to 74 '), in particular separated by at least 5 mm, and for each vent an additional material (7') forms a bridge between the lateral ends of the seal, in particular said seal material thus forming continuity of material.

Multiple liquid crystal variable diffusion glazing (100) according to the preceding claim, characterized in that the joint (7) is interrupted in its width by at least two vents (81 to 82) facing a first edge of the glazing and preferably by at least two other vents (83 to 84) facing a second edge opposite the first edge.

Liquid crystal variable diffusion multiple glazing (100) according to one of the preceding claims, characterized in that the seal (7) and / or additional material (7 ') is essentially organic, preferably epoxy resin. A method of producing a liquid crystal variable diffusion multiple glazing (100) according to claims 3 to 5 comprising the steps of:

the formation of the seal (7) comprising the application of the seal material (7) to the first float glass sheet (1) provided with the first electrode (3),

the liquid deposition of the liquid crystal layer (5) of an average thickness E on the first float glass sheet (1) provided with the first electrode (3) and possibly on the second float glass sheet (20); ) with the second electrode,

after the formation of the seal and the deposition of the liquid crystal layer, bringing the first and second glass sheets (1, 2) into contact,

characterized in that it comprises, before contacting the first and second glass sheets, the formation of one or more vents (81 to 84) of the gasket each defining the lateral ends (71 to 74 ') of gasket (7).

A process for producing a liquid crystal variable diffusion multiple glazing (100) according to claim 6, characterized in that the joint (7) being interrupted in its width by at least two vents (81 to 82) facing a first edge of the glazing and preferably by at least two other vents (83 to 84) facing a second edge opposite the first edge, and preferably, the assembly of the first and second sheets of glasses (1, 2) being made by calendering, these first and second edges correspond to the edges in the calendering direction.

Process for producing a liquid crystal variable diffusion multiple glazing unit according to claim 7, characterized in that the assembly of the first and second glass sheets being carried out in particular by pressing, the gasket of (7) interrupted in its width by minus two vents (81 to 82) next to a third edge of the glazing adjacent to the first edge and at least two other vents (83 to 84) facing a fourth edge opposite the third edge.

9. A method of producing a liquid crystal variable diffusion multiple glazing (100) according to one of claims 6 to 8 characterized in that it comprises the application of the additional material (7 '), forming a bridge between the lateral ends of the seal (71 to 74 ').

10. A method of producing a liquid crystal variable diffusion multiple glazing (100) according to the preceding claim characterized in that the additional material (7 ') is in said joint material (7), thus forming continuity of material, preferably substantially organic, especially epoxy resin.