CN1841168A - Sealing structure, sealing method, liquid crystal device and manufacturing method thereof, projector - Google Patents
Sealing structure, sealing method, liquid crystal device and manufacturing method thereof, projector Download PDFInfo
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- CN1841168A CN1841168A CN 200610071754 CN200610071754A CN1841168A CN 1841168 A CN1841168 A CN 1841168A CN 200610071754 CN200610071754 CN 200610071754 CN 200610071754 A CN200610071754 A CN 200610071754A CN 1841168 A CN1841168 A CN 1841168A
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Abstract
A liquid crystal device of the present invention includes a pair of substrates, a liquid crystal layer that is provided between the pair of substrates, a first seal material that is arranged along the periphery of the liquid crystal layer between the pair of substrates and seals the liquid crystal layer, and a second seal material that is arranged along the periphery of the liquid crystal layer between the pair of substrates and has water-hardening properties.
Description
Technical field
The present invention relates to hermetically-sealed construction, encapsulating method, liquid-crystal apparatus and manufacture method thereof and projector.
Background technology
As the optical modulator body of projection display devices such as liquid crystal projection apparatus and the liquid-crystal apparatus that is utilized, the circumference between a pair of substrate sets encapsulant, and portion is sealed with liquid crystal layer in the central.Be formed with the electrode that liquid crystal layer is applied voltage in the inboard of this a pair of substrate.Be formed with the alignment films of the orientation of control liquid crystal molecule when non-selection voltage applies in the inboard of this electrode.When applying based on non-selection voltage and the change in orientation of the liquid crystal molecule when selecting voltage to apply, modulated light source light is to make image light.
As alignment films, can utilize implemented the film that grinding (rubbing) is handled by the surface of the polymeric membrane of the polyimide formations such as (polyimide) of having added side chain alkyl (alkyl).So-called milled processed is meant by rub on the prescribed direction surface of polymeric membrane of the roller (roller) with soft cloth formation and makes macromolecular orientation in prescribed direction.By the intermolecular interaction of this orientation macromolecule and liquid crystal molecule, liquid crystal molecule is disposed along the orientation macromolecule.That is the liquid crystal molecular orientation when, non-selection voltage applies is on prescribed direction.And, provide pre-tilt (pretilt) by the side chain alkyl to liquid crystal molecule.
Under the situation of the liquid-crystal apparatus that will have organic alignment films as the optical modulator body of projector, high light or heat owing to from light source irradiation might make alignment films slowly decompose.After long-time the use, the possibility that the display quality that has liquid crystal molecule not to be arranged as the orientation control function of pre-tilt angle etc., liquid crystal molecule of expectation and liquid crystal projection apparatus reduces.
Thereby the employing of the alignment films that the inorganic material by photostability and superior for heat resistance is constituted is always studied.As the manufacture method of inorganic alignment film, schemes (for example opening clear 57-157214 communique with reference to the spy) such as ion beam sputtering or oblique side's vapour deposition method have been proposed.In these methods, the particle of the continuous incident inorganic material of substrate is formed the inorganic alignment film that the columnar structures by inorganic material constitutes with the incident angle of regulation.In liquid-crystal apparatus, liquid crystal molecule is along the columnar structures orientation of inorganic alignment film.That is to say, give orientation limitations and pre-tilt liquid crystal molecule by inorganic alignment film.
For sealing liquid crystal layer between a pair of substrate, need set encapsulant on the surface of inorganic alignment film.But, because the inorganic alignment film that is made of columnar structures is a porous matter, so might on the interface of encapsulant and inorganic alignment film, form bigger gap.Invade under the situation of liquid crystal layer by the outside of this gap at moisture or impurity etc., mainly hinder the orientation control function of the liquid crystal molecule in the liquid-crystal apparatus from liquid-crystal apparatus.This can cause the reduction of the reliability of liquid crystal projection apparatus.
Summary of the invention
The objective of the invention is to, a kind of hermetically-sealed construction, encapsulating method, liquid-crystal apparatus and manufacture method thereof that can reduce the possibility of intrusions such as moisture or impurity is provided.In addition, the projector that provides a kind of reliability superior is provided purpose.
Hermetically-sealed construction of the present invention is the hermetically-sealed construction at porous layer, wherein possesses: the 1st encapsulant, and it is provided in the surface of described porous layer; With the 2nd encapsulant, it is provided in the surface of described porous layer and has the hydraulicity.
Constitute according to this,, can prevent to be situated between by the intrusion of the moisture at the interface of the 1st encapsulant and porous layer and be situated between by the intrusion of the moisture of the inside of porous layer by the moisture absorption of the 2nd encapsulant.
Liquid-crystal apparatus of the present invention wherein possesses: a pair of substrate; Liquid crystal layer, it is configured between the described a pair of substrate; The 1st encapsulant, its be configured in described liquid crystal layer between described a pair of substrate around and seal described liquid crystal layer; With the 2nd encapsulant, its be configured in described liquid crystal layer between described a pair of substrate around and have a hydraulicity.
Constitute according to this,, can prevent that moisture from invading liquid crystal layer from the outside of liquid-crystal apparatus by the moisture absorption of the 2nd encapsulant.
Hope is formed with the alignment films of porous matter at the inner face of described substrate.
Constitute according to this, can prevent to be situated between by the moisture at the interface of the 1st encapsulant and porous layer to the intrusion of liquid crystal layer and be situated between by the intrusion of the moisture of the inside of alignment films to liquid crystal layer.
Wish that described the 2nd encapsulant is provided in the outside of described the 1st encapsulant.
According to this formation, be exposed to the outside and positively solidify the 2nd encapsulant by making the 2nd encapsulant.
Wish that described the 2nd encapsulant is made of the material that with the metal alkoxide is major component.
According to this formation, the 2nd encapsulant absorbs moisture and positively is cured.
The manufacture method of liquid-crystal apparatus of the present invention is the manufacture method that has sealed the liquid-crystal apparatus of liquid crystal layer between a pair of substrate, wherein has: the 1st encapsulant that is disposed around described liquid crystal layer, the operation of bonding described a pair of substrate; And the configuration on every side of the described liquid crystal layer between described a pair of substrate has the operation of the 2nd encapsulant of the hydraulicity.
Constitute according to this, provide a kind of configuration can prevent the liquid-crystal apparatus of moisture the intrusion of liquid crystal layer by the 2nd encapsulant.
Encapsulating method of the present invention wherein has: in the operation of the surface configuration encapsulant of described porous layer; With the configuring area of described encapsulant in described porous layer, give operation to the compatibility of described encapsulant.
According to this formation, easily encapsulant is filled into porous layer, therefore can prevent that moisture is via the intrusion via porous layer inside of the intrusion of encapsulant and porous layer and moisture.
The manufacture method of liquid-crystal apparatus of the present invention, it is the manufacture method that has sealed the liquid-crystal apparatus of liquid crystal layer between the 1st substrate and the 2nd substrate, wherein have: across being configured in described liquid crystal layer the 1st encapsulant on every side, the operation of bonding described the 1st substrate and described the 2nd substrate; With the operation of the configuring area of the described encapsulant of described the 1st substrate or described the 2nd substrate being given to the compatibility of described encapsulant.
Constitute according to this, substrate is good with respect to the wettability of encapsulant, thereby the possibility that makes moisture invade liquid crystal layer reduces.
Wish that the described configuring area of the described encapsulant in described the 1st substrate or the 2nd substrate only gives the compatibility to described encapsulant.
Constitute according to this, only make the regional activate of setting of encapsulant, thereby can prevent from the hygroscopic of zone in addition given.
The alignment films of the porous matter that hope forms on described the 1st substrate or the 2nd substrate is given the compatibility to described encapsulant.
Constitute according to this, alignment films is good to the wettability of encapsulant, thereby can prevent to be situated between by the moisture at the interface of encapsulant and alignment films to the immersion of liquid crystal layer and be situated between by the immersion to liquid crystal layer of the moisture of the inside of alignment films.
Described operation of giving the compatibility of encapsulant can have: to the operation of described the 1st substrate or described the 2nd substrate irradiates light; Described the 1st substrate or described the 2nd substrate are carried out the operation of Cement Composite Treated by Plasma; Or to the operation of the configuration of described the 1st substrate or described the 2nd substrate configuration surface modifier.
Liquid-crystal apparatus of the present invention uses the manufacture method of above-mentioned liquid-crystal apparatus.
Constitute according to this, can provide a kind of moisture etc. to immerse the little liquid-crystal apparatus of possibility of liquid crystal layer.
Projector of the present invention possesses described liquid-crystal apparatus as optical modulator body.
Constitute according to this, can provide a kind of reliability superior projector.
Description of drawings
Fig. 1 is the planimetric map of the tft array substrate of the liquid-crystal apparatus that relates to of the 1st embodiment.
Fig. 2 is the equivalent circuit diagram of liquid-crystal apparatus.
Fig. 3 is the key diagram of the planar structure of liquid-crystal apparatus.
Fig. 4 is the key diagram of the cross-section structure of liquid-crystal apparatus.
Fig. 5 A is the ion beam sputtering schematic representation of apparatus.
Fig. 5 B is the sectional side view that has formed the substrate of inorganic alignment film.
Fig. 6 A, 6B and 6C are the key diagrams of the hermetically-sealed construction that relates to of the 1st embodiment.
Fig. 7 A, 7B and 7C are the chemical formulas of organo-silicon compound.
Fig. 8 is the planimetric map of the tft array substrate of the liquid-crystal apparatus that relates to of the 2nd embodiment.
Fig. 9 A, 9B and 9C are the key diagrams of the encapsulating method that relates to of the 2nd embodiment.
Figure 10 is the summary pie graph of the pith of expression projector.
Embodiment
Below, with reference to accompanying drawing embodiments of the present invention are described.In each accompanying drawing that following explanation utilized,, suitably changed each parts the scale down of each parts for being made discernible size.In this manual, the liquid crystal layer side in each component parts of liquid-crystal apparatus is called the inboard; And its opposition side is called the outside.In addition, so-called " when non-selection voltage applies " and " when selecting voltage to apply ", be meant respectively " near applying in voltage is in the threshold voltage of liquid crystal layer " and " to liquid crystal layer apply the voltage ratio threshold voltage much higher in ".
(the 1st embodiment)
At first, the 1st embodiment of the present invention is described.Shown in Fig. 6 A～6C, the liquid-crystal apparatus that the 1st embodiment relates to, be circumference 10,20 of a pair of substrates be equipped with the 1st encapsulant 19 and in the central portion sealed the liquid-crystal apparatus 60 of liquid crystal layer 50.The outside at the 1st encapsulant 19 of 10,20 of substrates is equipped with the 2nd encapsulant 80 that is made of hydraulic material.And the liquid-crystal apparatus 60 of present embodiment is the permeation type liquid crystal device that has utilized active matrix (activematrix) mode of thin film transistor (TFT) as switch (switching) element (Thin Film Transistor, hereinafter referred to as TFT) element.
(liquid-crystal apparatus)
Fig. 1 is the planimetric map of tft array (array) substrate of liquid-crystal apparatus.Central portion at tft array substrate 10 is formed with image making zone 101.Circumference in this image making zone 101 is equipped with the 1st encapsulant 19.Be sealed with liquid crystal layer 50 (with reference to Fig. 4) in image making zone 101.Liquid crystal layer 50 direct coating of liquid crystalline and forming on substrate is not provided with the inlet of liquid crystal on the 1st encapsulant 19.Be equipped with the 2nd encapsulant 80 as the characteristic of present embodiment in the outside of the 1st encapsulant 19.In the outside of the 2nd encapsulant 80, be equipped with sweep trace described later is supplied with the scanning line driving element 110 of sweep signal and data line described later supplied with the data line driving element 120 of picture signal.The splicing ear 79 of the end of this driving element 110,120 and tft array substrate 10 is electrically connected by distribution 76.
On the subtend substrate 20 (with reference to Fig. 4) that tft array substrate 10 is pasted, be formed with common electrode 21.Common electrode 21 is formed on the almost whole zone in image making zone 101.Four jiaos of common electrode 21 are provided with conducting portion 70 between substrate.Conducting portion 70 and splicing ear 79 are electrically connected by distribution 78 between described substrate.Various signals by the outside input are fed into image making zone 101 via splicing ear 79, thereby drive liquid-crystal apparatus.
(equivalent electrical circuit)
Fig. 2 is the equivalent circuit diagram of liquid-crystal apparatus.The image making zone of permeation type liquid crystal device has and is configured to rectangular and has formed a plurality of points (dot) of pixel electrode 9 respectively.In the side of pixel electrode 9, be formed with TFT element 30 as the on-off element that carries out controlling to the energising of pixel electrode 9.Connecting data line 6a on the source electrode of TFT element 30.From described data line driving element to each data line 6a supply with picture signal S 1, S2 ..., Sn.
Connecting sweep trace 3a on the grid of TFT element 30.From above-mentioned scanning line driving element with predetermined timing to sweep trace 3a pulse type ground supply with sweep signal G1, G2 ..., Gm.Connecting pixel electrode 9 in the drain electrode of TFT element 30.If sweep signal G1, G2 by supplying with by sweep trace 3a ..., Gm, make as the only conducting during certain of the TFT element 30 of on-off element, then picture signal S1, the S2 that supplies with by data line 6a ..., Sn, be written to predetermined timing in the liquid crystal of each point via pixel electrode 9.
Write the specified level (level) in the liquid crystal picture signal S1, S2 ..., Sn, be held in the liquid crystal capacitance that is formed between pixel electrode 9 and the common electrode described later in during certain.The picture signal S1 that keeps in order to prevent, S2 ..., Sn leaks (leak), between pixel electrode 9 and electric capacity line 3b, be formed with and the memory capacitance 17 of liquid crystal capacitance configuration in parallel.If to the liquid crystal applied voltages signal, then the state of orientation of liquid crystal molecule changes.Its result makes the light source light that incides liquid crystal modulated, to make image light.
(planar structure)
Fig. 3 is the key diagram of the planar structure of liquid-crystal apparatus.In the liquid-crystal apparatus of present embodiment, a plurality of pixel electrodes 9 (representing its profile by dotted line 9a) are arranged as rectangular on tft array substrate.Pixel electrode 9 has rectangular shape and is made of the transparent conductivity material of indium tin oxide (Indium Tin Oxide, hereinafter referred to as ITO) etc.And, on tft array substrate, be provided with data line 6a, sweep trace 3a and electric capacity line 3b along the boundary in length and breadth of pixel electrode 9.In the present embodiment, the rectangular area that has formed each pixel electrode 9 is a little; And it all is the viewing area that each rectangular point is defended in configuration.
(cross-section structure)
Fig. 4 is the key diagram of the cross-section structure of liquid-crystal apparatus, also is the sectional side view of the A-A ' line of Fig. 3.As shown in Figure 4, the liquid-crystal apparatus 60 of present embodiment has: tft array substrate 10; Subtend substrate 20, itself and tft array substrate 10 subtends dispose; With liquid crystal layer 50, it is clamped between tft array substrate 10 and the subtend substrate 20.Tft array substrate 10 has: TFT element 30, pixel electrode 9 and the alignment films 16 of the base main body 10A that is made of the translucent material of glass or quartz etc., the inboard that is respectively formed at base main body 10A.Subtend substrate 20 has: the common electrode 21 and the alignment films 22 of the base main body 20A that is made of the translucent material of glass or quartz etc., the inboard that is respectively formed at base main body 20A.
On the surface of tft array substrate 10, be formed with the 1st photomask 11a described later and the 1st interlayer dielectric 12.On the surface of the 1st interlayer dielectric 12, form semiconductor layer 1a, and be formed centrally TFT element 30 in this semiconductor layer 1a being.With semiconductor layer 1a in the subtend part of sweep trace 3a on be formed with channel region 1a '.The distolateral formation source region of channel region 1a '; Another distolateral formation drain region.This TFT element 30 has adopted LDD (Lightly Doped Drain) structure.Therefore, on source region and drain region, formed the high relatively area with high mercury and relative low low concentration region (LDD zone) of impurity concentration respectively.That is to say, formed low concentration source region 1b and high concentration source region 1d in the source region; Low concentration drain region 1c and high concentration drain region 1e have been formed in the drain region.
On the surface of semiconductor layer 1a, be formed with gate insulating film 2.On the surface of gate insulating film 2, be formed with sweep trace 3a.With sweep trace 3a in the subtend of channel region 1a ' formed gate electrode on partly.In addition, on the surface of gate insulating film 2 and sweep trace 3a, formed the 2nd interlayer dielectric 4.The surface of the 2nd interlayer dielectric 4 has formed data line 6a.And by being formed at the contact hole 5 on the 2nd interlayer dielectric 4, data line 6a is connected with high concentration source region 1d.On the surface of the 2nd interlayer dielectric 4 and data line 6a, formed the 3rd interlayer dielectric 7.On the surface of the 3rd interlayer dielectric 7, formed pixel electrode 9.Via the contact hole 8 that is formed on the 2nd interlayer dielectric 4 and the 3rd interlayer dielectric 7, pixel electrode 9 is connected with high concentration drain region 1e.Form inorganic alignment film 16 in the mode that covers pixel electrode 9.By inorganic alignment film 16, the orientation of the liquid crystal molecule in the time of can limiting non-selection voltage and apply.
Also have, in the present embodiment, semiconductor layer 1a is set, thereby has formed the 1st storage capacitor electrode 1f by extension.In addition, gate insulating film 2 is set, thereby has formed deielectric-coating by extension.Formed the 2nd storage capacitor electrode by configuration electric capacity line 3b on the surface of dielectric film.Thus, constituted described memory capacitance 17.
On the surface of the base main body 10A corresponding, formed the 1st photomask 11a with the formation zone of TFT element 30.The light that the 1st photomask 11a prevents to incide liquid-crystal apparatus is invaded channel region 1a ', low concentration source region 1b and the low concentration drain region 1c of semiconductor layer 1a.
Formed the 2nd photomask 23 on the surface of base main body 20A in subtend substrate 20; The 2nd photomask 23 is parts of the light that prevents from the to incide liquid-crystal apparatus channel region 1a ', the low concentration source region 1b that invade semiconductor layer 1a, low concentration drain region 1c etc., and be set at when overlooking and semiconductor layer 1a overlapping areas in.Have again, on the almost whole zone on the surface of subtend substrate 20, formed the common electrode 21 that constitutes by electric conductors such as ITO.On the surface of common electrode 21, formed inorganic alignment film 22.The orientation of the liquid crystal molecule when applying by inorganic alignment film 22 restriction non-selection voltages.
Clamping by the liquid crystal layer 50 to formations such as row (nematic) type liquid crystal between tft array substrate 10 and subtend substrate 20.The nematic crystal molecule has positive dielectric constant anisotropy; It is along the substrate horizontal alignment, and vertical orientated along direction of an electric field when selecting voltage to apply when non-selection voltage applies.Have, the nematic crystal molecule has positive refractive index anisotropy again; Its birefringence and thickness of liquid crystal layer long-pending (retardation: postpone) Δ nd for example is 0.40 μ m (60 ℃) approximately.According to the orientation limitations direction of the alignment films 16 of tft array substrate 10 with according to the orientation limitations direction of the alignment films 22 of subtend substrate 20, be set to about 90 ° the state that twisted.Thus, the liquid-crystal apparatus 60 of present embodiment is carried out action with nematic mode (twisted nematic mode).
In the outside of each substrate 10,20, disposed polaroid 18,28 by the formations such as material of I that polyvinyl alcohol (PVA) (PVA) has been mixed.Also have, as preferably, polaroid 18,28 is installed on the supporting substrate that is made of high thermoconductivity materials such as sapphire glass or crystals, and separates configuration with liquid-crystal apparatus 60. Polaroid 18,28 has and absorbs the function that it absorbs axial rectilinearly polarized light, will see through through axial rectilinearly polarized light.The polaroid 18 of tft array substrate 10 is configured through the almost consistent mode of the axle and the orientation limitations direction of alignment films 16 with it.
Liquid-crystal apparatus 60 disposes subtend substrate 20 towards light source side.Have only in the light source light and see through polaroid 28 and incide liquid-crystal apparatus 60 with the consistent rectilinearly polarized light of axle that sees through of polaroid 28.In the liquid-crystal apparatus 60 when non-selection voltage applies, so that relatively the liquid crystal molecule of substrate horizontal alignment is thickness direction to liquid crystal layer 50 and has twisted about 90 ° spiral helicine mode and carry out laminated configuration.Incide the rectilinearly polarized light of liquid-crystal apparatus 60, penetrated from liquid-crystal apparatus 60 after about 90 ° of the optically-active.This rectilinearly polarized light, so because with polaroid 18 to see through axle consistent with a polaroid 18.Thus, carry out white demonstration (normally white mode) in the liquid-crystal apparatus when non-selection voltage applies 60.
In the liquid-crystal apparatus 60 when selecting voltage to apply, the relative substrate of liquid crystal molecule is vertical orientated.Incide the rectilinearly polarized light of liquid-crystal apparatus 60, penetrate from liquid-crystal apparatus 60 not by optically-active.Described rectilinearly polarized light is not so because see through polaroid 18 with the axle quadrature that sees through of polaroid 18.Deceive demonstration in the liquid-crystal apparatus 60 when thus, selecting voltage to apply.
(inorganic alignment film)
As mentioned above, be formed with inorganic alignment film 16,22 in the inboard of each substrate 10,20.Below, the inorganic alignment film 16 of tft array substrate 10 is described.The inorganic alignment film 22 of subtend substrate 20 also has identical therewith formation.
Fig. 5 A is the ion beam sputtering schematic representation of apparatus.Ion beam sputtering device S100 possesses: off-gas pump S4, its control vacuum chamber S3 and internal pressure thereof; Substrate holder (holder) S5, it is at vacuum chamber S3 internal fixation substrate 10; Target (target) S2, it is to substrate 10 ejection sputtering particles; With ion gun S1, it is to target S2 irradiation ion beam.Ion gun S1 is connected with gas supply source S13.Filament (filament) S11 and extraction electrode S12 are being set in the inside of ion gun S1.
Utilize ion beam sputtering device 10 to form inorganic alignment film, can carry out following order.At first, substrate 10 is fixed on the substrate holder S5 in the vacuum chamber S3, and is reduced pressure in the inside of vacuum chamber S3 by off-gas pump S4.Then, to supplying with inert gas such as argon gas in the ion gun S1, and filament S11 is applied voltage so that thermoelectron produces by gas supply source S13.So the thermoelectron of generation and the inert gas of importing bump and produce plasma on ion gun S1.Then, S12 applies ion accelerating voltage to extraction electrode, by plasma the ion that produces is quickened.Thus, from ion gun S1 irradiation ion beam.By the target S2 of ion beam irradiation, to form the sputtering particle that material constitute of substrate 10 ejections by inorganic alignment film.This sputtering particle is deposited on the substrate 10, forms inorganic alignment film on substrate 10.
Pressure in the vacuum chamber S3 is preferably 5 * 10
-1Below the Pa, more preferably 5 * 10
-2Below the Pa.If this hypertonia then reduces the rectilinear propagation of the sputtering particle shone.The temperature of substrate 10 is preferably below 150 ℃, more preferably below 100 ℃, further is preferably 50～80 ℃.By substrate 10 is remained under the lower temperature, thereby can suppress to be adsorbed on the phenomenon (migration) that the sputtering particle of substrate 10 moves from the position of initial absorption.Be applied to the ion accelerating voltage on the extraction electrode S12, be preferably 400～3000V, more preferably 800～2000V.If ion accelerating voltage is low excessively, then sputter rate reduces; And if ion accelerating voltage is too high, then be difficult to form uniform film.
Fig. 5 B is the sectional side view that has formed the substrate of inorganic alignment film.If to substrate 10 continuous incident sputtering particles, then sputtering particle is piled into the batter post shape and is formed the columnar structures 16a of inorganic material with the incident angle of constant.Incalculably form this columnar structures 16a on the surface of substrate 10, thereby constitute inorganic alignment film 16.Also have, by adjusting the target S2 shown in Fig. 5 A and the angle of substrate 10, make sputtering particle with the incident angle of regulation to substrate 10 incidents, thereby can give the angle of inclination of regulation to the columnar structures 16a shown in Fig. 5 B.In liquid-crystal apparatus, liquid crystal molecule is orientated along columnar structures 16a.That is to say that by inorganic alignment film 16, the liquid crystal molecular orientation when non-selection voltage is applied is limited in prescribed direction, and gives pre-tilt to liquid crystal molecule.
Also have, also can adopt following formation: by forming a plurality of dip plane on the basilar memebrane of inorganic alignment film surface in advance, on described surface, form inorganic alignment film by described sputtering method, thereby make the shape of described a plurality of dip plane be communicated to the surface of inorganic alignment film.Have again, also can after having formed inorganic alignment film, carry out ion milling (ion milling), on the surface of inorganic alignment film, form the recess of directivity with regulation with predetermined angular incident ion bundle by described sputtering method.Have again, also can carry out ion milling on the basilar memebrane surface of inorganic alignment film in advance, form inorganic alignment film with described sputtering method then, further carry out ion milling once more and form recess on the surface of inorganic alignment film on its surface.Under any situation, can both provide and positively to give the inorganic alignment film of the pre-tilt angle of expectation to liquid crystal molecule.
(hermetically-sealed construction)
Fig. 6 A～6C is the key diagram of the hermetically-sealed construction that relates to of present embodiment, also is the sectional side view of the B-B line of Fig. 1.Also have, as shown in Figure 1, be equipped with the 1st encapsulant 19 at the circumference of tft array substrate 10, and portion is sealed with liquid crystal layer in the central.
Shown in Fig. 6 C, formed described inorganic alignment film 16,22 in the inboard of each substrate 10,20.Be equipped with the 1st encapsulant 19 around the liquid crystal layer 50 between this inorganic alignment film 16,22.The 1st encapsulant 19 is made of the material that has mixed the material of hardening agent or further mixed the uv curing resin of acrylic acid (acrylic) etc. in the heat-curing resin of epoxy (epoxy) etc.Have again, for the liquid crystal bed thickness of realizing stipulating (cell gap), the distance piece 19a of dispersing ball in the 1st encapsulant 19.
Have again, around the liquid crystal layer 50 in 16,22 of inorganic alignment films, the outside of the 1st encapsulant 19 set the 2nd encapsulant 80.The hydraulic material that the 2nd encapsulant 80 solidifies by absorbing moisture constitutes.As this hydraulic material, wish to adopt to comprise the material of the metal alkoxide of element silicon as major component.That is, will use as host by the organo-silicon compound of the represented poly-dialkoxy siloxane of the chemical formula of Fig. 7 A, the poly-dimethoxysiloxane of Fig. 7 B or the tetraalkoxysilane of Fig. 7 C etc.Also have, for hydraulic material, remove host with fit on crosslinking chemical and curing catalysts, also cooperated pigment or aggregate as required.Particularly, as hydraulic material, can adopt the テ リ オ ス コ one ト NP-3600QD of emerging system of Co., Ltd.'s day.This is to contain the weight of silicon composition at the silicon solution more than 90%, is the coating solution that forms amorphous glass-film of hard at normal temperatures.
As an example, to tetraalkoxysilane (Si (OR)
4) adopt, the consolidated structures of halogen (X) when adopting as curing catalysts described as host.
(1)
Shown in (1) formula, BX
4-As easy as rolling off a log and the Si of ion replaces and becomes SiX
4-Ion, and hydrolysis reaction shown in (2) formula of acceleration and the dehydration condensation shown in (3) formula.Its result is cured at normal temperatures and generates glass (SiO
2).At this, the water (H that is consumed in (1) formula and (2) formula
2O) then many than the water that is generated in (3) formula.Thus, this material can absorb moisture and be cured.
Then, utilize Fig. 6 A～6C, the manufacture method of the liquid-crystal apparatus that present embodiment is related to describes.At first, as shown in Figure 6A, surface coated the 1st encapsulant 19 that is being formed at the inorganic alignment film 16 on the substrate 10.
Then, shown in Fig. 6 B, at the inboard coating of liquid crystalline of the 1st encapsulant 19 and form liquid crystal layer 50.The coating of this liquid crystal can utilize drop ejection method to wait and carry out.Then paste tft array substrate 10 and subtend substrate 20 and the 1st encapsulant 19 is solidified.Because the 1st encapsulant 19 be by heat-curing resin with and/or uv curing resin constitute, so carry out heat treated with and/or ultraviolet treatment with irradiation and solidify the 1st encapsulant 19.Thus, the relative position of tft array substrate 10 and subtend substrate 20 is fixed, and realized the liquid crystal bed thickness of stipulating by the distance piece 19a that is dispersed in the 1st encapsulant 19.Also have, also can in the 1st encapsulant, liquid crystal injecting port be set, after having pasted substrate 10,20, inject liquid crystal.
Then, shown in Fig. 6 C, be equipped with the 2nd encapsulant 80 in the outside of the 1st encapsulant 19.Particularly, the side from a pair of substrate 10,20 pasted across the 1st encapsulant 19 utilizes divider (dispenser) to the gap of substrate 10,20 coating hydraulic material.Because substrate 10,20 is about a few μ m at interval, so the hydraulic material of coating is filled in the gap of substrate 10,20 by capillarity.Absorb moisture and be cured at normal temperatures by this hydraulic material, thereby set the 2nd encapsulant 80 at the circumference of 10,20 of substrates.Also have, as preferably, coating the 2nd encapsulant 80 under low viscous state, and the 2nd encapsulant 80 is filled in the gap of columnar structures 16a of inorganic alignment film 16.Have again, paste subtend substrate 20 again after also can not only being coated with the 1st encapsulant 19 to the surface of tft array substrate 10 but also being coated with the 2nd encapsulant 80.Have again, also can implement dried and make its curing the hydraulic material that is coated with.
The above finishes the liquid-crystal apparatus that present embodiment relates to.
But, because the inorganic alignment film 16 that is made of columnar structures 16a like that shown in Fig. 5 B is a porous matter, so might between the 1st encapsulant 19 and substrate 10, form the gap.Particularly might form bigger gap at the interface of the 1st encapsulant 19 and inorganic alignment film 16.If by this gap, moisture or impurity etc. immerse liquid crystal layer from the outside of liquid-crystal apparatus, then can hinder the various functions of liquid-crystal apparatus.Particularly, if immerse as the water of polarizability molecule in the liquid crystal of holding polarization structure then that the orientation of liquid crystal takes place is bad.
To this, the hermetically-sealed construction of present embodiment, have liquid crystal layer 50 in 10,20 of a pair of substrates around set the formation of the 2nd encapsulant 80 with hydraulicity.Constitute according to this, the moisture that immerses liquid crystal layer 50 from the outside of liquid-crystal apparatus 60 is absorbed by the 2nd encapsulant 80, thus, has reduced the possibility that moisture immerses the inside of liquid crystal layer 50.Its result can keep the various functions of liquid-crystal apparatus 60 steadily in the long term.Particularly, prevent to immerse in the liquid crystal of holding polarization structure and the orientation condition of poor of liquid crystal takes place as the water of polarizability molecule.By this liquid-crystal apparatus 60 is adopted as optical modulator body, thereby improve the reliability of liquid crystal projection apparatus.
Have, the hermetically-sealed construction of present embodiment has the formation that has set the 2nd encapsulant 80 in the outside of the 1st encapsulant 19 again.According to this formation, because the 2nd encapsulant 80 exposes externally, so the 2nd encapsulant 80 positively is cured.Have again because for liquid crystal layer 50 the 1st encapsulant 19 and the same contact the in the past, so the reduction of reliability that prevents the deterioration of the liquid crystal layer 50 that the influence by the 2nd encapsulant 80 causes and follow the liquid-crystal apparatus 60 of this deterioration.Also have,, also can set the 2nd encapsulant 80 in the inboard of the 1st encapsulant 19 if it is no problem to contrast these viewpoints.
The hermetically-sealed construction of described present embodiment, be by the 2nd encapsulant 80 polishings moisture cutting function among the various sealing functions expected of the 1st encapsulant 19.In order to strengthen this moisture cutting function, also can add the 3rd encapsulant.Have, the function of other that expected for polishing the 1st encapsulant 19 also can be added the 3rd encapsulant again.Described each encapsulant is as long as each condition is allowed also and can be set with arbitrary order.
On the other hand, even in the 2nd encapsulant 80, also can satisfy under the situation of sealing function that the 1st encapsulant 19 has or reliability etc., also can replace 19 of the 1st encapsulants to set the 2nd encapsulant 80.
(the 2nd embodiment)
Then, the 2nd embodiment of the present invention is described.Shown in Fig. 9 A～9C, the manufacture method of the liquid-crystal apparatus that the 2nd embodiment relates to, be the manufacture method that between tft array substrate 10 (the 1st substrate) and subtend substrate 20 (the 2nd substrate), has sealed the liquid-crystal apparatus 60 of liquid crystal layer 50, wherein have: the operation of coming adhesive substrate 10 and substrate 20 across the 1st encapsulant 19; With the configuring area of encapsulant 19 in the surface of inorganic alignment film 16,22 on being formed at substrate 10,20, give operation to the compatibility of encapsulant 19.Also have,, omit or simplify its detailed description the part of the formation identical with the 1st embodiment.
(liquid-crystal apparatus)
Fig. 8 is the planimetric map of the tft array substrate of liquid-crystal apparatus.Central portion at tft array substrate 10 has formed image making zone 101.Circumference in this image making zone 101 has set encapsulant 19.In image making zone 101, be sealed with liquid crystal layer 50 (with reference to Fig. 9 C).Liquid crystal layer 50 direct coating of liquid crystalline and forming on substrate; The inlet of liquid crystal layer is not set on encapsulant 19.In the outside of sealing material 19, the data line driving element 120 that sweep signal is supplied to the scanning line driving element 110 of sweep trace described later and picture signal is supplied to data line described later is installed.This driving element 110,120, with the splicing ear 79 of the end of tft array substrate 10, be electrically connected by distribution 76.
Being pasted on the subtend substrate 20 of tft array substrate 10 (with reference to Fig. 9 C), formed common electrode 21.Common electrode 21 almost is formed in the whole zone in image making zone 101.Four jiaos at common electrode 21 are provided with conducting portion 70 between substrate.Conducting portion 70 and splicing ear 79 are electrically connected by distribution 78 between substrate.Supply to image making zone 101 by being situated between by splicing ear 79, thereby drive liquid-crystal apparatus from the various signals of outside input.
(method for making of liquid-crystal apparatus)
Fig. 9 A～9C is the key diagram of the manufacture method of the liquid-crystal apparatus that relates to of present embodiment, also is the sectional side view of the B-B line of Fig. 8.Also have, as shown in Figure 8, be equipped with encapsulant 19 at the circumference of FTF array base palte 10, and portion is sealed with liquid crystal layer in the central.
In the present embodiment, shown in Fig. 9 A, surface treatment is implemented in the zone that sets of the encapsulant in the substrate 10 19 (with reference to Fig. 9 B); Shown in Fig. 9 B, set encapsulant 19 like that; Shown in Fig. 9 C, paste subtend substrate 20 like that; Thereby form liquid-crystal apparatus 60.
At first, shown in Fig. 9 A, like that substrate 10 is implemented surface treatment.As mentioned above, because be formed with inorganic alignment film 16, so this inorganic alignment film 16 is implemented surface treatment on the surface of substrate 10.At this, only surface treatment is implemented in the zone that sets of encapsulant 19 as preferred.Special preferred surface is handled the formation zone that does not arrive liquid crystal layer 50 (with reference to Fig. 9 C).Therefore, implement surface treatment the setting the area configurations mask (mask) 90 beyond the zone of encapsulant 19.As described mask 90, can utilize photoresist (photoresist) or hardmask (hard mask) etc.By the zone that sets only implementing surface treatment at encapsulant 19, thus can prevent encapsulant 19 set zone beyond the zone by activate, and be endowed hydroscopicity.Particularly by preventing to give hydroscopicity, thereby reduced the possibility that moisture or impurity etc. immerse liquid crystal layers 50 to the formation zone of liquid crystal layer 50.
Described surface treatment is preferably irradiates light and carries out.Particularly, preferably it utilizes irradiation ultraviolet radiations such as UV-lamp.Be adsorbed on the lip-deep organism of substrate 10 etc. by the ultraviolet light degradation removal, make the surface activation of formed inorganic alignment film 16 on the substrate 10.Its result, the compatibility of 16 pairs of encapsulants 19 of raising inorganic alignment film.Also have, also can replace ultraviolet ray, or while irradiation ultraviolet radiation, electron ray or laser etc.
Have again, also can carry out Cement Composite Treated by Plasma as surface treatment.These treatment conditions are: for example under the situation of having utilized oxygen, plasma power (power) is that the flow of 50～1000W, oxygen is that the transporting velocity of 50～100ml/min, substrate article on plasma body sparking electrode is that the temperature of 0.5～10mm/sec, substrate is 70～90 ℃.Plant by the activation that excites that oxygen gas plasmaization is formed oxonium ion or oxygen radical (radical) etc.Make the surface activation of inorganic alignment film 16 by this lip-deep organism that excites the activation kind decompose to remove to be adsorbed on substrate 10 etc.Its result, the compatibility of 16 pairs of encapsulants 19 of raising inorganic alignment film.Also have, replace oxygen also can utilize inert gases such as argon gas, nitrogen.In addition, Cement Composite Treated by Plasma both can also can be carried out in atmospheric pressure in a vacuum.Perhaps, also can utilize the ozone gas that generates by oxygen plasma etc.
Have again as surface treatment, also can adopt HMDS ((CH
3)
3SiNHSi (CH
3)
3Hexamethyldisilazane).Particularly, be full of in the HMDS steam in the container and on the surface of inorganic alignment film 16, be coated with HMDS by substrate 10 is exposed to.Its result, the compatibility of 16 pairs of encapsulants of raising inorganic alignment film.
Have again as surface treatment, also can or carry out the gas phase film forming at substrate 10 coating surface modifier.As surface modifier, adopt to combine with the silanol group (Si-O-H) on the surface of inorganic alignment film 16 and form the material of unimolecular film.Particularly, need only the silane coupling agent of employing chlorosilane or amino silane, alkoxy silane, silazane etc.Have again, also can adopt the alcohols of decyl alcohol or 18 alcohol (carbon chain length), isopropyl alcohol etc.Have again, also can adopt to have the surfactant-based of hydrophobicity base.Under any situation, because the hydroxyl on the surface of inorganic alignment film 16 can be replaced into the surface that hydrophobic group comes modified inorganic alignment films 16, so can improve compatibility with the encapsulant 19 that constitutes by resin material etc.
Be through with after the surface treatment of inorganic alignment film 16, remove mask 90.
Then, shown in Fig. 9 B, coating encapsulant 19 on the surface of having implemented surface-treated inorganic alignment film 16.As encapsulant 19, can adopt the material that in heat-curing resins such as epoxy, has mixed the material of hardening agent or further mixed the uv curing resin of acrylic acid etc.Also can make the electroconductive particle that is used for guaranteeing with the conducting of subtend substrate be distributed to encapsulant 19 in addition.Sealing material 19 utilizes divider etc. to be coated on the circumference of substrate 10.
But, because the inorganic alignment film 16 shown in Fig. 5 B is made of the columnar structures 16a that inorganic material constitutes, so lack compatibility with the encapsulant 19 that constitutes by resin material etc.Therefore, might form bigger gap at the interface of inorganic alignment film 16 and encapsulant 19.In addition, be difficult to gap packing matcrial 19 to the columnar structures 16a of inorganic alignment film 16.And exist by these gaps, moisture or impurity etc. immerse the possibility of liquid crystal layer from the outside of liquid-crystal apparatus.
To this, in the present embodiment shown in Fig. 9 B, the compatibility of 16 pairs of encapsulants 19 of inorganic alignment film is higher.Therefore, the encapsulant 19 that is coated with is in the expansion of the surface wettability of inorganic alignment film 16, and is filled in the gap of columnar structures 16a of inorganic alignment film 16.Thus, to invade the possibility of inside of liquid crystal layer from the interface of inorganic alignment film 16 and encapsulant 19 or from the gap of the columnar structures 16a of inorganic alignment film 16 etc. lower for moisture or impurity etc.
Also have, as preferably, under the state that waits the viscosity that makes encapsulant 19 to reduce by heating and encapsulant 19 is coated with.Thus, can be to the gap of the columnar structures 16a of inorganic alignment film 16 packing matcrial positively.
Thereafter, such inboard coating of liquid crystalline shown in Fig. 9 C at encapsulant 19.The coating of liquid crystal can utilize drop ejection method to wait and carry out.Then, contraposition is carried out in the position of tft array substrate 10 and subtend substrate 20, adhesive substrate and encapsulant 19 is solidified.Also have, as preferably, even, also implement described surface treatment in advance the zone that sets of the encapsulant in the subtend substrate 20 19.
According to the above, finish the liquid-crystal apparatus that present embodiment relates to.
As described in detail above, according to the manufacture method of the liquid-crystal apparatus of present embodiment, can reduce the possibility that moisture or impurity etc. are invaded the inside of liquid crystal layers 50.Its result keeps the various functions of liquid-crystal apparatus 60 steadily in the long term.Particularly, prevent to immerse in the liquid crystal of holding polarization structure and the orientation condition of poor of liquid crystal takes place as the water of polarizability molecule.By this liquid-crystal apparatus 60 is adopted as the reliability that optical modulator body improves liquid crystal projection apparatus.
More than also having, though, also exist only to form inorganic alignment film and in the regional situation that does not form inorganic alignment film of setting of encapsulant in the formation zone of liquid crystal layer not only to the formation of liquid crystal layer 50 zone but also to being illustrated in all situations that forms inorganic alignment film 16,22 in the surface of substrate 10,20.That is to say, setting of encapsulant the nesa coating of ITO etc. is exposed, and the electroconductive particle that is dispersed in the encapsulant is touched on the nesa coating, to guarantee the situation of the conducting between substrate.Even in this case,, nesa coating is constituted with columnar structures if form ITO etc. with sputtering method.Thus, might on the interface of nesa coating and encapsulant, form bigger gap.Thereby, even do not form under the situation of inorganic alignment film in the zone that sets of encapsulant, the manufacture method of the liquid-crystal apparatus that also preferably suitable present embodiment relates to.In view of the above, can prevent that the interface of nesa coating and encapsulant from forming the situation in bigger gap, and reduce the possibility that moisture or impurity etc. are invaded the inside of liquid crystal layer.
(projector)
Then, utilize Figure 10 that projector of the present invention is described.Figure 10 is the summary pie graph of the pith of expression projector.This projector is the instrument that the liquid-crystal apparatus that described each embodiment relates to is possessed as optical modulator body.
In Figure 10, the 810th, light source; 813, the 814th, dichronic mirror (dichroic mirror); 815, the 816, the 817th, catoptron; The 818th, the incident lens; The 819th, relay lens, the 820th, exit lens; 822, the 823, the 824th, the optical modulator body that constitutes by liquid-crystal apparatus of the present invention; The 825th, quadrature color separation water chestnut mirror (cross dichroic prism); The 826th, projecting lens.Light source 810 constitutes by metal halide lamp (metal halide lamp) with the reverberator (reflector) 812 of the light of lamp reflection.
Three coloured light by after each optical modulator body 822,823,824 modulation incide quadrature color separation water chestnut mirror 825.This quadrature color separation water chestnut mirror 825 is parts of having pasted 4 right angle water chestnut mirrors; Its interface X word shape formed with the multilayer dielectric film of reflection to red light with the multilayer dielectric film of blu-ray reflection.By these multilayer dielectric films three coloured light are synthesized, and formed the light of color display.The light that is synthesized projects to screen 827 by the projecting lens 826 as projection optical system, shows after image is amplified.
Described projector possesses the liquid-crystal apparatus of described each embodiment as optical modulator body.The liquid-crystal apparatus of each embodiment is because have the inorganic alignment film of photostability and superior for heat resistance, so less than situation about being worsened by high light or the hot alignment films that causes from light source irradiation.And, moisture etc. by encapsulant and inorganic alignment film the interface or to be immersed in the possibility of liquid crystal layer by formed gap, the inside of inorganic alignment film lower.Thus, this projector is being kept the orientation control function of the liquid crystal molecule in the liquid-crystal apparatus steadily in the long term and is being had higher reliability.
Also have, technical scope of the present invention is not to be defined in above-mentioned embodiment, in the scope that does not break away from purport of the present invention, also comprises the mode that has increased various changes in the above-described embodiment.For example, though be that example is illustrated with the liquid-crystal apparatus that possessed TFT as on-off element in the embodiment, also the present invention can be applicable to the liquid-crystal apparatus that has possessed thin film diode two-terminal type elements such as (Thin Film Diode) as on-off element.In addition, though be that example is illustrated with the permeation type liquid crystal device in the embodiment, also the present invention can be applicable in the reflective liquid crystal device.Have again, though (Twisted Nematic: twisted nematic) liquid-crystal apparatus that works of pattern is that example is illustrated, and also the present invention can be applicable to the liquid-crystal apparatus that works with VA (Vertical Alignment: vertical orientated) pattern with TN in the embodiment.Have again,, also the present invention can be applicable to the projection display device or the direct viewing type display device of one-board though in embodiment, 3 board-like projection display devices (projector) are illustrated as an example.
Have again, also liquid-crystal apparatus of the present invention can be applicable to projector electronic device in addition.As this concrete example, can enumerate mobile phone.This mobile phone has possessed the liquid-crystal apparatus that described each embodiment or its variation relate in display part.Have again, as other electronic device, can also enumerate: IC-card, video camera, personal computer, Helmet Mounted Display (head mounted display), further the facsimile unit of subsidiary Presentation Function, the view finder of digital camera, portable TV, DSP device, PDA, electronic notebook, electric light bulletin board, propaganda bulletin are arranged with display etc.
Claims (16)
1, a kind of hermetically-sealed construction, it wherein possesses at porous layer:
The 1st encapsulant, it is provided on the surface of described porous layer; With
The 2nd encapsulant, it is provided on the described surface of described porous layer, and has the hydraulicity.
2, a kind of liquid-crystal apparatus wherein possesses,
A pair of substrate;
Liquid crystal layer, it is configured between described a pair of substrate;
The 1st encapsulant, its be configured in described liquid crystal layer between described a pair of substrate around, and seal described liquid crystal layer; With
The 2nd encapsulant, its be configured in described liquid crystal layer between described a pair of substrate around, and have the hydraulicity.
3, liquid-crystal apparatus according to claim 2, wherein,
The inner face of described substrate is formed with the alignment films of porous matter.
4, according to claim 2 or 3 described liquid-crystal apparatus, wherein,
Described the 2nd encapsulant is provided in the outside of described the 1st encapsulant.
5, according to each described liquid-crystal apparatus in the claim 2 to 4, wherein,
Described the 2nd encapsulant is by the material of metal alkoxide as major component constituted.
6, a kind of manufacture method of liquid-crystal apparatus, it is the manufacture method that has sealed the liquid-crystal apparatus of liquid crystal layer between a pair of substrate, wherein has:
Across the 1st encapsulant, paste the operation of described a pair of substrate; With
Configuration has the operation of the 2nd encapsulant of the hydraulicity around the described liquid crystal layer between described a pair of substrate.
7, the manufacture method of liquid-crystal apparatus according to claim 6, wherein,
The operation of described configuration the 2nd encapsulant has: from the side of the described a pair of substrate pasted across described the 1st encapsulant, inject the operation of hydraulic material to the gap of described a pair of substrate.
8, a kind of encapsulating method, it wherein has at porous layer:
The operation of configuration encapsulant on the surface of described porous layer; With
The configuring area of the described encapsulant in described porous layer is given the operation to the compatibility of described encapsulant.
9, a kind of manufacture method of liquid-crystal apparatus, it is the manufacture method that has sealed the liquid-crystal apparatus of liquid crystal layer between the 1st substrate and the 2nd substrate, wherein has:
Make the operation of described the 1st substrate and described the 2nd substrate sticking across the 1st encapsulant; With
The configuring area of the described encapsulant in described the 1st substrate or described the 2nd substrate is given the operation to the compatibility of described encapsulant.
10, the manufacture method of liquid-crystal apparatus according to claim 9, wherein,
Only the described configuring area of the described encapsulant in described the 1st substrate or described the 2nd substrate is given the compatibility to described encapsulant.
11, according to the manufacture method of claim 9 or 10 described liquid-crystal apparatus, wherein,
Give compatibility to the alignment films that is formed on the porous matter on described the 1st substrate or the 2nd substrate to described encapsulant.
12, according to the manufacture method of each described liquid-crystal apparatus in the claim 9 to 11, wherein, described operation of giving the compatibility of encapsulant has: to the operation of described the 1st substrate or described the 2nd substrate irradiates light.
13, according to the manufacture method of each described liquid-crystal apparatus in the claim 9 to 11, wherein, described operation of giving the compatibility of encapsulant has: the operation of described the 1st substrate or described the 2nd substrate being carried out Cement Composite Treated by Plasma.
14, according to the manufacture method of each described liquid-crystal apparatus in the claim 9 to 11, wherein, described operation of giving the compatibility of encapsulant has: the operation of configuration surface modifier on described the 1st substrate or described the 2nd substrate.
15, a kind of liquid-crystal apparatus, wherein,
Use the manufacture method of each described liquid-crystal apparatus in the claim 9 to 14 to make.
16, a kind of projector, wherein,
As optical modulator body, possesses in the claim 2 to 5 liquid-crystal apparatus described in each or the claim 15.
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| JP2005092269 | 2005-03-28 | ||
| JP2005092269 | 2005-03-28 | ||
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| JP2005329859 | 2005-11-15 |
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| US5543186A (en) * | 1993-02-17 | 1996-08-06 | E. Khashoggi Industries | Sealable liquid-tight, thin-walled containers made from hydraulically settable materials |
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