CA1260374A - Method and apparatus for applying an anti-lacerative plastic layer to glass - Google Patents

Method and apparatus for applying an anti-lacerative plastic layer to glass

Info

Publication number
CA1260374A
CA1260374A CA000479716A CA479716A CA1260374A CA 1260374 A CA1260374 A CA 1260374A CA 000479716 A CA000479716 A CA 000479716A CA 479716 A CA479716 A CA 479716A CA 1260374 A CA1260374 A CA 1260374A
Authority
CA
Canada
Prior art keywords
sheet
glass
glass substrate
substrate sheet
laceration
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired
Application number
CA000479716A
Other languages
French (fr)
Inventor
Siegfried H. Herliczek
Charles E. Ash, Jr.
Stephen P. Bartus, Jr.
Ronald L. Toth
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Pilkington North America Inc
Original Assignee
Libbey Owens Ford Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Libbey Owens Ford Co filed Critical Libbey Owens Ford Co
Application granted granted Critical
Publication of CA1260374A publication Critical patent/CA1260374A/en
Expired legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10009—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets
    • B32B17/10036—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets
    • B32B17/10045—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the number, the constitution or treatment of glass sheets comprising two outer glass sheets with at least one intermediate layer consisting of a glass sheet
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10165—Functional features of the laminated safety glass or glazing
    • B32B17/10293—Edge features, e.g. inserts or holes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/1055—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer
    • B32B17/10761—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing characterized by the resin layer, i.e. interlayer containing vinyl acetal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10816—Making laminated safety glass or glazing; Apparatus therefor by pressing
    • B32B17/10825—Isostatic pressing, i.e. using non rigid pressure-exerting members against rigid parts
    • B32B17/10834—Isostatic pressing, i.e. using non rigid pressure-exerting members against rigid parts using a fluid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B17/00—Layered products essentially comprising sheet glass, or glass, slag, or like fibres
    • B32B17/06—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material
    • B32B17/10—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin
    • B32B17/10005—Layered products essentially comprising sheet glass, or glass, slag, or like fibres comprising glass as the main or only constituent of a layer, next to another layer of a specific material of synthetic resin laminated safety glass or glazing
    • B32B17/10807—Making laminated safety glass or glazing; Apparatus therefor
    • B32B17/10889—Making laminated safety glass or glazing; Apparatus therefor shaping the sheets, e.g. by using a mould
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/36—Layered products comprising a layer of synthetic resin comprising polyesters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/554—Wear resistance
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2307/00—Properties of the layers or laminate
    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
    • B32B2307/58—Cuttability
    • B32B2307/581—Resistant to cut
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2367/00—Polyesters, e.g. PET, i.e. polyethylene terephthalate
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B2605/00—Vehicles

Abstract

ABSTRACT OF THE DISCLOSURE
The present invention concerns a unique method for producing an anti-lacerative glass assembly wherein a plastic composite anti-laceration sheet is to be bonded to a glass substrate sheet. The plastic anti-laceration sheet includes an inner layer of polyvinyl butyral adapted to abut the glass substrate sheet, an intermediate layer of poly-ester, and an outer layer of abrasion resistant material. A
glass cover sheet having substantially the same curvature as the glass substrate sheet is utilized to press the anti-laceration sheet into bonding engagement with the glass sub-strate sheet. In accordance with the present invention, the bonding operation is accomplished by heating the laminated glass assembly a predetermined temperature in the range of 285° F to 305° F. It has been found that such a temperature must be sufficiently high to cause the intermediate layer of polyester to bond to the inner layer of polyvinyl butyral, and to cause the inner layer of polyvinyl butyral to bond to the glass substrate sheet, and must be sufficiently low to prevent crazing of the abrasion resistant coating. The present invention also concerns the use of a unique vacuum ring construction which is mounted about the periphery of the laminated assembly and is utilized to de-air the assembly. The vacuum ring is provided with a check valve to maintain the vacuum within the ring during periods wherein it is disconnected from a vacuum source. Further, the method of the present invention includes the step of re-moving a selected portion or portions of the anti-laceration sheet after it has been bonded to the glass substrate sheet to provide an exposed glass surface for use in mounting the glass assembly into an associated frame.

Description

The present invention relates generally to a method and apparatus for applying a layer of plastic material to a glass sheet and, in particular, to a method for producing an anti-lacerative window assembly for use in automotive vehicles.
It has been found that the addition of a plastic layer bonded to the inboard glass surfase of a conventional laminated windshleld can further increase the safety effec~iveness of the windshield. This plastic layer has typically been termed an anti-laceration shield since it has been found that the additional plastic layer will appreciably reduce the number and severity of lacerative in~uries to persons thrown against the windshield under all impact conditions. Further, it has been found that the anti-laceration shield, when produced under certain conditions of manufacture, improves the ability of the laminated windshield to decelerate movement of a person thrown against the windshield, while also increasing the penetration resistance of the windshield as compared to conventional laminated windshields. Also, the laceration shield reduces the amount of fly~ng glass and thus the in~ury to car occupants as a result of objects that may be thrown against the windshield from overpasses or elsewhere outside the vehicle.
An example of one type of anti-lacerative windshield is disclosed in United States Patent No.
4,242,403. In this patent, the laceration sh~eld includes a penetration resisting multi-layer body consisting of an inner layer of relatively soft, extensible plastic material Sr~

such as polyvinyl butyral, which is adhered to the inboard surface of the windshield, an intermediate layer of more durable plastic such as polyester, and an outer coating of an abrasion resistant material. Another type of anti-lac~rative windshield is disclosed in United States Patent No. 3,808,077 wherein a single layer of polyurethane is utilized as an anti-laceration shield.
While the effectiveness of a laminated windshield having an anti-laceration shield is obvious, very few vehicles utilize such a windshield. The chief reason for this limited use has been the difficulty experienced in trying to manufacture a windshield with an anti-laceration shield on a production basis. In the automotive industry, the standard for windshields is very high, especially as to optical qualities, and it has been very difficult to manufacture a windshield having an anti-laceration shield which is free of optical defects. Even when the individual sheets of the laminated assembly are free from optical defects before bonding them together, it is difficult to ~oin them and preserve the optical qualities.
The present invention concerns a unlque method for producing an anti-lacerative glass assembly. The initial step involves assembling a glass substrate sheet having a predetermined curvature, an anti-laceration sheet and a glass cover sheet having substantially the same curvature as a glass substrate sheet into a stacked arrangement. In the preferred embodiment of the invention, the anti-laceration sheet is a plastic composite sheet which includes an inner layer of polyvinyl butyral adapted to abut the glass substrate sheet, an intermediate layer of polyester, and an outer layer of an abrasion resistant material adapted to abut the gla~s cover sheet. Once the stacked arrangement of individual laminae have been assembled, a vacuum ring is placed about the peripheral edges of the laminated glass assembly and is coupled to a vacuum source to de-air the assembly and urge the individual laminae toward one another.
Next, the assembly is placed in an autoclave unit wherein the laminated glass assembly is heated to a predetermined temperature in the range of 285~ F to 305 F, while simultaneously pressure is applied to the exterior surfaces of the laminated assembly. It has been discovered that, when a plastic composite anti-laceration sheet of the type described above is utilized, the autoclave bonding temperature is very critical. For example, the autoclave temperature must be sufficiently high to enable the intermediate polyester layer to properly bond to the inner polyvinyl butyral layer, and the temperature must be sufficlently low to prevent crazing of the abrasion resistant coating~
Once a predetermined temperature and a predetermined pressure have been reached in the autoclave, these levels are maintained for a predetermined time period.
At the end of this time period, the temperature in the autoclave is reduced while the pressure is maintained at the predetermined level. After the temperature has fallen below a predetermined point such as 125 F9 the pressure then can be reduced, and the laminated assembly can be removed from the autoclave.
The present invention also concerns the use of a vacuum ring having a unique construction. The vacuum ring is provided with a check valve means such that the vacuum ring can be disconnected from a vacuum source while mainta1ning ~2~3~

the vacuum within the ring. If desired, the vacuum ring can then be reconnected to the vacuum source.
The method of the present invention can further include the step of, subsequent to producing an anti-lacerative glass assembly, removlng a selected portlon or portions of the anti-laceration sheet from the glass substrate sheet to define an exposed glass surface which can be used either to mount the windshield within an associated frame, or to mount a rear view mirror assembly.
Alternatively, the invention concerns th~ use of a unique cover sheet utilized to position the anti-laceration sheet in a selected position on the glass sheet to wh~ch the anti-laceration sheet is to be bonded.
According to the present invention, there is provided a method of producing an anti-lacerative glass assembly comprising the steps of:
a) assembling into a stacked arrangement individual laminae including a glass substrate sheet having a predetermined curvature, a plastic composite anti-laceration sheet having one surface abutting the glass substrate sheet, and a glass cover sheet having substantially the same curvature as the glass substrate sheet and abutting the opposite surface of the composite anti-laceration sheet, thereby producing a laminated glass assembly, the plastic composite anti-laceration sheet including an inner layer of polyvinyl butyral adapted to abut the glass substrate sheet, an intermediate layer of polyester, and an outer layer of an abrasion resistant material adapted to abut 3~ the glass cover sheet;

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b) urging the individual laminae of th~ glass assembly toward one another;
c) simultaneously with step (b), heating ~he laminated glass assembly to a predetermined temperature ln the range o~ 285F to 305~, for a predetermined period and then subsequently reducing the temperature, said predetermined temperature being sufficiently high to cause the intermediate layer of polyester to bond to the inner layer of polyvinyl butyral and to cause the inner layer of polyvinyl butyral to bond to the glass substrate sheet and being sufficiently low to prevent crazing of the abrasion resistant coating; and d) removing the glass cover sheet from the laminated glass assembly to produce the anti-lacerative glass assembly.
Also9 according to this invention, there is provided an apparatus intended for use in bonding a plastic sheet to a glass substrate sheet having a predetermined curvature and having an outer periphery larger than the perlphery of the plastic sheet, comprising: a glass cover sheet havlng substantially the same curvature as the glass substrate sheet and adapted to abut an outwardly facing surface of the plastic sheet, said glass cover sheet lncluding a positioning means located on one surface thereof for positioning and maintaining at least a portion of the marginal edge of the plastic sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet, said positioning means adapted to sealingly contact the glass substrate sheet to prevent the plastic sheet from flowing across and bonding to a predetermined portioll of the marginal edge surface of the glass substrnte 33~

sheet contacted by said positioning means during the bonding operation.
In the accomanying drawings:
Fig. 1 is a rear elevational view of a laminated window assembly produced by the method of the present invention;
Fig. 2 is a fragmentary sectional view taken along the line 2-2 of Fig. l;
Fig. 3 is an enlarged sectional view taken along the line 3-3 of Fig. 2 and illustrating the individual laminae which comprise the plastic composite anti-laceration sheet;
Fig. 4a is a fragmentary sectional view illustrating the individual laminae which comprise the first sub-assembly utilized in the method of the present invention;
Fig. 4b is a fragmentary sectional view illustrating the individual laminae which comprise the second sub-assembly utilized in the method of the present invention;
Fig. 5 is a plan view of the laminated glass assembly having a vacuum ring attached thereto which is utilized to evacuate any air spaces between the individual laminae;
Fig. 6 is a fragmentary sectional view taken along the line 6-6 of Fig. 5 and illustrating the laminated glass assembly having the vacuum ring positioned about the peripheral edge thereof; and Fig. 7 is a diagram illustrating the preferred pressure-temperature sequence wh$ch occurs during the autoclave operation.

It should be noted at the outset of this descrlption that, whlle the embodiment of the invention illLlstrated in the drawings and described herein concerns an anti-lacerative window assembly consisting of two laminated sheets of glass, it will be appreciated that the method and apparatus of the present invention can readily be adapted to produce an anti-lacerative window consisting of a single sheet of glass. Also~ while the preferred embodiment of the invention is described as a vehicle windshield, it will be appreciated that the anti-lacerative window can also be used as a side or rear vehicle window, or as a window in other types of safety applications.
Referring to Figs. 1 through 3, there is shown one type oE laminated glass assembly, such as an automotive windshield 10, which can be produced by the method of the present invention. The windshield 10 includes two sheets of glass 12 and 14 which are bonded together by means of a plastic interlayer 16 positioned therebetween. The plastic interlayer 16 is typically a sheet of relatively soft extensible plastic material in the range of 0.025 to 0.040 inch thick and capable of being bonded to a glass surface.
In the preferred embodiment of ~he invention, the plastic interlayer 16 is a sheet of polyvinyl butyral approximately 0.030 to 0.0375 inch thick. Also, the glass sheets 12 and 14 are preferably sheets of float glass, in thicknesses in the range of 0.070 inch to 0.125 inch. In ~he preferred embodiment of the invention, the glass sheets 12 and 14 are approximately 0.100 inch thick. IE a single ply anti-lacerative window is to be produced, the single sheet of glass is typically in the range of 0.090 to 0.150 inch thick.

)37~

Additionally, the glass sheet 14, which is adapted to face the interior of the vehicle, has a plas-tic composite anti-laceration sheet 18 bonded to the in-board glass surface 14a. As shown in the enlarged sec-tional view of Fig. 3, the anti-laceration sheet 18 is a three layer composite sheet comprising a layer 20 of a relatively soft extensible plastic material, a layer 22 . of a more durable plastic material, and an outer CQating or layer 24 of an abrasion resistant plastic material.
In the preferred embodiment of the invention, the soft extensible plastic layer 20 is approximately 0.015 inch thick and can be polyvinyl butyral, for example, while the more durable plastic layer 22 is approximately 0.002 to 0.007 inch thick and can be a heat treated polyester, for example. if a single ply anti-lacerative window is to be produced, the inner layer of polyvinyl butyral is typically 0.030-0.045 inch thick.
The abrasion resistance coating 24 is relative-ly thin as compared to the layers 20 and 22 and can be cured, organopolysiloxane compound reinforced with silica.
More specifically, the plastic layers 20 and 22 and the abrasion resistant coating 24 may be of the types des- ~
cribed in United States Patents 3,900,673; 4,059,469;
4,112,171; 4,177,315; and 4,242,403. A plastic composite anti-laceration sheet of the type utilized in the prefer-red embodiment of the invention is available from the E.I. Du Pont De Nemours and Company, Wilmington, Delaware, U.S.A.
As previously mentioned, the present invention concerns a unique method for producing a laminated glass ! assembly of the type as illustrated in Figs. l through 3.
In the method of the present invention, the individual 3~*

laminae which comprise the laminated assembly are first assembled in two separate sub assemblles. The flrst sub-assembly 26, illustrated in Fig. 4a, comprises a stacked arrangement which includes the pair of glass sheet 12 and 14 having the plastic interlayer 16 positioned therebetween.
The second sub-assembly 28, illustrated in Fig. 4b, includes the plastic composite anti-laceration sheet 18 which is placed on a surface 30a of a glass cover sheet 30 having substantially the same curvature as the glass sheets 12 and 14. The composite anti-laceration sheet is placed on the cover sheet 30 such that the abrasion rèsistance coating 24 abuts the surface 30a. Typically, the cover sheet 30 is formed of a sheet of float glass. As will be discussed, the cover sheet 30 is utilized to produce a laminated glass assembly of high optical quality by assisting in bonding the anti-laceration sheet 18 to the outer surface 14a of the glass sheet 14.
It has been dlscovered that, in producing an anti-laceration windshield of the type shown in Figs. 1 through 3, it is desirable that the anti-laceration sheet 18 not cover selected portions of the inboard glass surface 14a such that those selected portions provide an exposed glass surface. For example, in Fig. 1, the marginal edge of the laceration sheet 18 is spaced inwardly from the marginal edge of the glass sheet 14 to define a peripheral edge portion 14b having an exposed glass surface. It has been discovered that such an exposed glass surface is desirable when mounting the windshield in an associated vehicle frame, since the adhesives typically utilized to secure the windshield within the frame have been found to adhere more readily to a glass surface than to the plastic surface of ~2~3~

the anti~laceration sheet. Also, in Fig. 1, a circular cutout is provided in the anti-laceration sheet 18 to define a circular portion 14c havlng an exposed glass surface. The circular portion 14c can be utllized for securing a rear view mirror mount assembly to the windshield.
In addition to providing a better adhesive surface, the selected exposed glass surfaces also provide other advantages. For example, in the event a windshield must be temporarily removed from the vehicle, or a mirror mount must be replaced, any damage to the anti-laceration sheet is avoided. Also, if the vehicle window frame or the mlrror mount was adhered directly to the anti-laceration sheet, any separation of the frame or mirror mount from the windshield tends to separate the anti-laceration sheet from the glass substrate sheet, thereby causing distortion in those areas.
While the anti-laceration sheet 18 can be bonded to the entire glass surface 14a, and selected portions of the laceration sheet can subsequently be removed from the glass surface 14a to provide the selected exposed glass surface portions 14b and 14c, the removal of selected portions of the anti-laceration sheet can be a relatively time consuming task and can effect damage to the glass substrate sheet. Preferably, the anti-laceration sheet is initially precut to predetermined dimensions such that, when the anti-laceration sheet is properly positioned and bonded to the glass sheet 14, the selected portions of the glass surface 14a will remain exposed and there is no need for any subsequent trimming and removal of portions of the anti-laceration sheet.

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In order to assist in positioning the anti-laceration sheet 18 on the glass surface 14a, the method of the present invention utilizes a cover sheet 30 of a unique design. More specifically, the glass cover sheet 30 of the present invention includes a positioning means such as a dam or gasket 32, for example, which is secured about the peripheral edges of the surface 30a to define a boundary within which the anti-laceration sheet 18 is to be placed. The gasket 32 is constructed of a resilient material having a thickness approximately equal to the overall thickness of the anti-laceration sheet. While the gasket 32 can be constructed of cork, silicone, fiber-reinforced silicon, or rubber, it has been found desirable to construct the gasket of Teflon*.
Typically, the surface of the Teflon* gasket which is to be secured to the glass surface of the cover sheet is specially treated to assist in the adhesion of the gasket to the cover sheet. It has been found that a conventional epoxy provides a suitable means for securing the Teflon~ gasket to the glass surface.

The location on the cover sheet surface 30a to which the gasket 32 is secured corresponds to the peripheral edge portion 14b on the glass surface 14a which is to remain exposed. In addition to the peripheral gasket 32, a circular gasket 34 is secured to the surface 30a at the location corresponding the exposed circular portion 14c for the mirror mount assembly.
Thus, in the preferred embodiment of the invention, the plastic composite anti-laceration sheet 18 is precut to dimensions which enable the sheet l~ to be placed on the cover sheet surfac~ 30a within the boundary of the peripheral gasket 32.
MoreoverJ as shown in Fig. 4b, a circular cutout portion 18a ~ Trade mark of E.I. Dupont de Nemours ~ CoO

LCM:jj 11 ~2~

is provided in the anti-laceration sheet at the location corresponding to the circular gasket 34.
It has been found that, prior to placing the anti-laceration sheet 18 on the surface 30a of the glass cover sheet 30/ it is desirable to apply a release agent to the surface 30a to enable the cover sheet 30 to be easily removed from the anti-laceration sheet after the anti-laceration sheet has been bonded to the glass sheet 14.
- While the release agent can be a conventional silicone wax, it is preferable to utili~e a silane having the formula R -Si(OR)4 wherein R is an alkyl group and n is a number from 1 to 3. In this connection, good results have been obtained with the use of an alkyl-trialkoxy silane and particularly n-propyl-trimenthoxy silane, and dialkyl-dialkoxy silanes, particularly diethyl-diethoxy silane.
After the two individual sub-assemblies as illustrated in Figs. 4a and 4b are produced, the two individual sub-assemblies are assembled to produce a laminated glass assembly whereln the polyvinyl butyral layer of the anti-laceration sheet 18 of the second sub-assembly 28 abuts the outwardly facing glass surface 14a of the first sub-assembly 26. Prior to assembling the two sub-asse~blies, it is preferable to apply a primer to the outer glass surface 14a to assist in bonding the anti-laceration sheet 18 to the glass sheet 14. The primer can be a silane solution which includes 0.5 to 3% by volume of silane in a solvent such as isopropyl alcohol. The silane can be gamma-aminopropyltriethoxysilane which is available from Union Carbide Corporation, Danbury, Connecticut, U.S.A. under the trade designation A-1100.

~L~ r~

After the first and second sub-assemblles have been positioned together to form the laminated glass assernbly, the air spaces betwsen the individual lamlnae are evacuated to urge the individual laminae toward one another.
This can be accomplished by positioning a vacuum ring 36, as shown in Figs. 5 and 6, about the peripheral edge of the laminated glass assembly. The vacuum ring 36 dcfines an interior chamber 36a in communication with a flexible conduit 37 which is adapted to be coupled to a vacuum source (not shown). The vacuum ring 36 can ~e constructed of silicone or neoprene3 for example.
The method of the present invention utilizes a vacuum ring having a unique construction. More specifically, the vacuum ring is provided with a quick~disconnect coupling 38 having a check valve means incorporated therein. Such a coupling is commercially available from Crawford Fitting Co. of Solon, Ohio, U.S.A., as Part No. SS-QC-4-D-4HC. After the vacuum ring 36 has been positioned about the laminated glass assembly and coupled to a vacuum source for a predetermined period of time to de-air the assembly, the vacuum ring can be disconnected from the vacuum source, and the check valv~
means will continue to maintain the vacuum in the chamber 36a.
The laminated assembly having the vacuum ring attached is then placed in an autoclave unit (not shown) which is designed to apply pressure to the exterior surfaces of the laminated assembly, while simultaneously heating the entire laminated assembly to a predetermined temperature to cauge the plastic interlayer 16 to bond to the pair of glass sheets 12 and 14 and ~o cause the PVB layer of the anti-laceration sheet 18 to bond to the surface 14a of the glass sheet 14. In the event a plastic composite anti-laceration sheet of the type shown in Fig. 3 i8 used, the autoclave operation also causes the intermediate polyester layer 22 to bond to the inner polyvinyl butyral layer 20. While in the autoclave, the vacuum ring 36 can be connected to the vacuum source to maintain the vacuum within the chamber 36a during the bonding operation.
Typically, the pressure in the autoclave is in the range of 20~ to 275 psi, while the temperature is in the range of 250 F to 325 F. This temperature and pressure are typically maintained for approximately twenty to thirty minutes to assure an effective bonding between the individual laminae.
It has been discovered that, in the event a plastic composite anti-laceration sheet of the type shown in Fig. 3 is used, the autoclave bonding temperature is very critical. For example, the autoclave temperature must be sufficiently high to enable the intermediate polyester layer 22 to properly bond to the inner polyvinyl butyral layer 20, and the temperature must be sufficiently low to prevent crazing of the abrasion resistance coating 240 It has been found that an autoclave temperature in the range of 285 F
to 305 F provides satisfactory results. For optimum reeults, a temperature of approximately 295 F should be used.
Fig. 7 illustrates a time diagram of the preferred temperature/pressure sequence for the autoclave bonding operation of an anti-laceration window assembly utilizing the composite anti-laceration sheet of Fig. 3. As shown Ln Fig. 7, after the laminated assembly has been placed in the 37~

autoclave and the autoclave has been sealed, the pressure and temperature is increased until the pressure reaches 250 p.s.i. and the temperature reaches 295 F. The pressure and temeprature are then maintained at these levels ~or approximately 25 minutes.
After the 25 minute period, the temperature is reduced while the pressure is maintained at 250 p. 8 .i. to ensure that the surface 30a of the cover sheet 30 is maintained in complete contact with the anti-laceration sheet. Otherwise 9 reducing the pressure before the laminated assembly has sufficiently cooled can cause the cover sheet to pull away from the anti-laceration sheet in certain areas, thereby causing increased distortion in those areas. After the temperature has fallen below a predetermined point, the pressure can then be reduced, and the laminated assembly can be removed from the autoclave.
It has been found that allowing the temperature to fall below 125 F before reducing the pressure provides satisfactory results.
After the laminated assembly has been removed from the autoclave, the vacuum ring 36 is removed. Next, the cover sheet 30 can be removed from the laminated assembly such that the remaining portion of the laminated assembly constitutes the anti-laceration windshield 10 of Fig. 1.
In accordance with the provisions of the patent statutes, the principle and mode of operation of the present invention have been illustrated and described in what is considered to represent the preferred embodiment. ~owever, it should be understood that the present invention can be ~L2~

practiced otherwise than as specifically illustrated and described wlthout departing from the scope of the following claims.

Claims (27)

  1. THE EMBODIMENTS OF THE INVENTION IN WHICH AN EXCLUSIVE
    PROPERTY OR PRIVILEGE IS CLAIMED ARE DEFINED AS FOLLOWS:
    l. A method of producing an anti-lacerative glass assembly comprising the steps of:
    a) assembling into a stacked arrangement individual laminae including a glass substrate sheet having a predetermined curvature, a plastic composite anti-laceration sheet having one surface abutting the glass substrate sheet, and a glass cover sheet having substantially the same curvature as the glass substrate sheet and abutting the opposite surface of the composite anti-laceration sheet, thereby producing a laminated glass assembly, the plastic composite anti-laceration sheet including an inner layer of polyvinyl butyral adapted to abut the glass substrate sheet, an intermediate layer of polyester, and an outer layer of an abrasion resistant material adapted to abut the glass cover sheet;
    b) urging the individual laminae of the glass assembly toward one another;
    c) simultaneously with step (b), heating the laminated glass assembly to a predetermined temperature in the range of 285°F to 305°F, for a predetermined period and then subsequently reducing the temperature, said predetermined temperature being sufficiently high to cause the intermediate layer of polyester to bond to the inner layer of polyvinyl butyral and to cause the inner layer of polyvinyl butyral to bond to the glass substrate sheet and being sufficiently low to prevent crazing of the abrasion resistant coating; and d) removing the glass cover sheet from the laminated glass assembly to produce the anti-lacerative glass assembly.
  2. 2. The method according to claim 1 wherein step (b) includes the step of applying a predetermined pressure in the range of 225 to 275 psi for a second predetermined time period to the exterior surfaces of the laminated assembly to urge the individual laminae toward one another and then subsequently reducing the pressure.
  3. 3. The method according to claim 2 wherein said predetermined temperature and pressure are both maintained for a predetermined time period in the range of 20 to 30 minutes.
  4. 4. The method according to claim 2 wherein, prior to reducing the predetermined pressure applied to the laminate glass assembly, the laminated glass assembly is cooled to a temperature less than 125° F.
  5. 5. The method according to claim 2 including, simultaneously with step (b), the step of evacuating spaces between the individual laminae to further urge the individual laminae toward one another.
  6. 6. The method according to claim 1 wherein said predetermined temperature is approximately 295° F.
  7. 7. The method according to claim 2 wherein said predetermined pressure is approximately 250 p.s.i.
  8. 8. The method according to claim 3 wherein said predetermined time period is approximately 25 minutes.
  9. 9. A method of producing an anti-lacerative glass assembly comprising the steps of:
    a) assembling into a stacked arrangement individual laminae including a glass substrate sheet, having a predetermined curvature, a plastic anti-laceration sheet having one surface abutting the glass substrate sheet, and a glass cover sheet having substantially the same curvature as the glass substrate sheet and abutting the opposite surface of the anti-laceration sheet, thereby producing a laminated glass assembly;
    b) placing a vacuum ring about the peripheral edges of the laminated glass assembly, the vacuum ring including a conduit adapted to be coupled to a vacuum source, the conduit provided with a check valve means for maintaining the vacuum within the ring when the conduit is disconnected from the vacuum source;
    c) connecting the conduit to a vacuum source to urge the individual laminae toward one another and evacuate air spaces between the individual laminae;
    d) disconnecting the conduit from the vacuum source wherein the check valve means provided in the conduit maintains the vacuum within the ring;
    e) placing the laminated glass assembly having the vacuum ring attached thereto within an autoclave unit;
    f) reconnecting the conduit of the vacuum ring to a vacuum source;
    g) pressurizing and heating the laminated glass assembly within the autoclave to cause the anti-laceration sheet to bond to the glass substrate sheet; and h) removing the glass cover sheet from the laminated glass assembly to produce the anti-lacerative glass assembly.
  10. 10. A method of producing an anti-lacerative glass assembly comprising the steps of:
    a) assembling into a stacked arrangement individual laminae including a glass substrate sheet, having a predetermined curvature, a plastic anti-laceration sheet having one surface abutting the glass substrate sheet, and a glass cover sheet having substantially the same curvature as the glass substrate sheet and abutting the opposite surface of the anti-laceration sheet, thereby producing a laminated glass assembly;
    b) urging the individual laminae of the glass assembly toward one another;
    c) simultaneously with step (b), heating the glass assembly to a predetermined temperature to cause the anti-laceration sheet to bond to the glass substrate sheet;
    d) removing the glass cover sheet from the laminated glass assembly to produce an anti-lacerative glass assembly; and e) removing a selected portion or portions of the anti-laceration sheet from the glass substrate sheet to produce an anti-lacerative glass assembly wherein at least a portion of the surface of the glass substrate sheet to which the anti-laceration sheet was bonded becomes an exposed glass surface.
  11. 11. The method according to claim 10 including, subsequent to step (e), applying an adhesive to the exposed glass surface.
  12. 12. The method according to claim 10 wherein the selected portion of the anti-laceration sheet removed in step (e) includes a peripheral edge portion of the anti-laceration sheet, thereby providing an exposed glass surface along the peripheral edge of the glass substrate sheet.
  13. 13. The method according to claim 12 including, subsequent to step (e), securing the anti-lacerative glass assembly to an associated frame by applying an adhesive to the exposed glass surface.
  14. 14. The method according to claim 10 wherein the selected portion of the anti-laceration sheet removed in step (e) defines an exposed glass surface for adhesively securing a mirror mount thereto.
  15. 15. A method of producing an anti-lacerative glass assembly comprising the steps of:
    a) providing a glass substrate sheet having a predetermined curvature;
    b) providing a plastic anti-laceration sheet having an outer periphery smaller than the outer periphery of the glass substrate sheet;
    c) providing a glass cover sheet having substantially the same curvature as the glass substrate sheet and having a positioning means located on one surface thereof;
    d) assembling into a stacked arrangement individual laminae including the glass substrate sheet, the plastic anti-laceration sheet abutting an outwardly facing surface of the glass substrate sheet, and the glass cover sheet abutting an outwardly facing surface of the anti-laceration sheet, the positioning means of the glass cover sheet adapted to position and maintain at least a portion of the marginal edge of the anti-laceration sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet and to sealingly contact the glass substrate sheet to prevent the anti-laceration sheet from flowing across and bonding to a predetermined portion of the marginal edge surface of the glass substrate sheet contacted by the positioning means during the bonding operation;
    e) urging the individual laminae of the laminated glass assembly toward one another;
    f) simultaneously with step (e), heating the laminated glass assembly to a predetermined temperature to cause the anti-laceration sheet to bond to the glass substrate sheet; and g) removing the glass cover sheet from the laminated glass assembly to produce an anti-lacerative glass assembly wherein the predetermined portion of the marginal edge of the glass substrate sheet which was contacted by the positioning means is an exposed glass surface.
  16. 16. An apparatus intended for use in bonding a plastic sheet to a glass substrate sheet having a predetermined curvature and having an outer periphery larger than the periphery of the plastic sheet, comprising: a glass cover sheet having substantially the same curvature as the glass substrate sheet and adapted to abut an outwardly facing surface of the plastic sheet, said glass cover sheet including a positioning means located on one surface thereof for positioning and maintaining at least a portion of the marginal edge of the plastic sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet, said positioning means adapted to sealingly contact the glass substrate sheet to prevent the plastic sheet from flowing across and bonding to a predetermined portion of the marginal edge surface of the glass substrate sheet contacted by said positioning means during the bonding operation.
  17. 17. The apparatus according to claim 16 wherein the glass substrate sheet and said glass cover sheet are non-planar.
  18. 18. The apparatus according to claim 16 wherein said positioning means is constructed of TEFLON.
  19. 19. The apparatus according to claim 16 wherein said positioning means has a thickness substantially equal to the thickness of the plastic sheet.
  20. 20. The apparatus acording to claim 19 wherein said positioning means surrounds the entire periphery of said one surface of said cover sheet and the plastic sheet is sized such that said positioning means maintains the entire marginal edge of the plastic sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet.
  21. 21. A method of producing an anti-lacerative glass assembly comprising the steps of:
    a) providing a glass substrate sheet having a predetermined curvature;
    b) providing a plastic anti-laceration sheet;
    c) removing a predetermined cutout portion from the interior of the plastic anti-laceration sheet;

    d) providing a glass cover sheet having substantially the same curvature as the glass substrate sheet and having a gasket means located on one surface thereof;
    e) assembling into a stacked arrangement individual laminae including the glass substrate sheet, the plastic anti-laceration sheet abutting one surface of the glass substrate sheet, and the glass cover sheet abutting an outwardly facing surface of the anti-laceration sheet, the gasket means of the cover sheet adapted to be inserted into the cutout provided in the anti-laceration sheet and to sealingly contact the glass substrate sheet to prevent the anti-laceration sheet from flowing onto and bonding to a predetermined interior portion of the one surface of the glass substrate sheet contacted by the gasket means during the bonding operation;
    f) urging the individual laminae of the laminated glass assembly toward one another;
    g) simultaneously with step (f), heating the laminated glass assembly to a predetermined temperature to cause the anti-laceration sheet to bond to the glass substrate sheet; and h) removing the glass cover sheet from the laminated glass assembly to produce an anti-lacerative glass assembly wherein the predetermined interior portion of the one surface of the glass substrate sheet which was contacted by the gasket means is an exposed glass surface.
  22. 22. An apparatus intended for use in bonding a plastic sheet to a glass substrate sheet having a predetermined curvature, the plastic sheet provided with a predetermined cutout portion removed from the interior thereof, said apparatus comprising: a glass cover sheet having substantially the same curvature as the glass substrate sheet and adapted to abut an outwardly facing surface of the plastic sheet, said glass cover sheet including a gasket means located on one surface thereof for insertion into the cutout provided in the plastic sheet, said gasket means adapted to sealingly contact the glass substrate sheet to prevent the plastic sheet from flowing onto and bonding to a predetermined interior portion of the one surface of the glass substrate sheet contacted by said gasket means during the bonding operation.
  23. 23. The apparatus according to claim 22 wherein the glass substrate sheet and said glass cover sheet are non-planar.
  24. 24. The apparatus according to claim 22 wherein said gasket means is constructed of
  25. 25. The apparatus according to claim 22 wherein said gasket means has a thickness substantially equal to the thickness of the plastic sheet.
  26. 26. The apparatus according to claim 22 wherein the plastic sheet has an outer periphery smaller than the periphery of the glass substrate sheet and said apparatus further includes a positioning means located on said one surface of said glass cover sheet for positioning at least a portion of the marginal edge of the plastic sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet, said positioning means adapted to sealingly contact the glass substrate sheet to prevent the plastic sheet from flowing across and bonding to a predetermined portion of the marginal edge surface of the glass substrate sheet contacted by said positioning means during the bonding operation.
  27. 27. The apparatus according to claim 26 wherein said positioning means surrounds the entire periphery of said one surface of said cover sheet and the plastic sheet is sized such that said positioning means maintains the entire marginal edge of the plastic sheet in inwardly spaced relationship relative to the marginal edge of the glass substrate sheet.
CA000479716A 1984-04-27 1985-04-22 Method and apparatus for applying an anti-lacerative plastic layer to glass Expired CA1260374A (en)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US60487684A 1984-04-27 1984-04-27
US604,876 1984-04-27
US71706085A 1985-03-28 1985-03-28
US717,060 1985-03-28

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EP (1) EP0179862A4 (en)
KR (1) KR930011145B1 (en)
AU (1) AU579371B2 (en)
BR (1) BR8506693A (en)
CA (1) CA1260374A (en)
DE (1) DE3590207T1 (en)
ES (1) ES8606127A1 (en)
GB (1) GB2176438B (en)
NL (1) NL8520086A (en)
SE (2) SE8506058L (en)
WO (1) WO1985005073A1 (en)

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JPS61500603A (en) * 1983-12-08 1986-04-03 リビ−−オ−ウェンズ−フォ−ド・カンパニ− Vacuum equipment for laminated glass production
GB8619464D0 (en) * 1986-08-09 1986-09-17 Glaverbel Bending thermoplastics sheets
DE3632472A1 (en) * 1986-09-24 1988-03-31 Flachglas Ag MOTORCYCLE DISC
CH673435A5 (en) * 1987-05-27 1990-03-15 Fela Planungs Ag
FR2616426B1 (en) * 1987-06-11 1992-10-16 Quimal International Ltd COMPOSITE GLAZING HAVING IMPACT RESISTANCE PROPERTIES
KR100372374B1 (en) * 2000-10-30 2003-02-19 조동하 Manufacture method of bulletproof glass
KR100705654B1 (en) * 2004-12-31 2007-04-10 박복만 Safety Complex Glass for Decoration
US9391124B2 (en) 2013-07-02 2016-07-12 Samsung Display Co., Ltd. Organic light emitting diode display
KR101646447B1 (en) 2015-02-09 2016-08-05 현대자동차주식회사 A vacuum ring and a method for producing laminated assembly with it
JP7188132B2 (en) * 2019-01-25 2022-12-13 Ａｇｃ株式会社 Method for manufacturing vehicle structure, and method for manufacturing transparent substrate with protective film

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US2382956A (en) * 1942-10-21 1945-08-21 Libbey Owens Ford Glass Co Process of manufacture of safety glass
NL209656A (en) * 1955-08-19 1900-01-01
US3208899A (en) * 1962-09-11 1965-09-28 Du Pont Laminating frame
LU52726A1 (en) * 1966-12-30 1968-08-05
FR2085238B2 (en) * 1970-03-16 1974-08-09 Saint Gobain Pont A Mousson
US3808077A (en) * 1971-09-16 1974-04-30 Ppg Industries Inc Method for laminating plastic to glass employing glass mold
FR2247348B1 (en) * 1973-10-15 1977-05-27 Saint Gobain
US4242403A (en) * 1976-08-02 1980-12-30 Libbey-Owens-Ford Company Automotive glazing units and method of producing the same
US4065340A (en) * 1977-04-28 1977-12-27 The United States Of America As Represented By The National Aeronautics And Space Administration Composite lamination method
JPS61500603A (en) * 1983-12-08 1986-04-03 リビ−−オ−ウェンズ−フォ−ド・カンパニ− Vacuum equipment for laminated glass production

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KR860700020A (en) 1986-01-31
ES8606127A1 (en) 1986-04-01
DE3590207T1 (en) 1986-05-15
SE8506058D0 (en) 1985-12-20
NL8520086A (en) 1986-03-03
SE8700879L (en) 1987-03-03
SE8700879D0 (en) 1987-03-03
ES542608A0 (en) 1986-04-01
GB2176438B (en) 1988-09-28
WO1985005073A1 (en) 1985-11-21
EP0179862A1 (en) 1986-05-07
GB8530652D0 (en) 1986-01-22
SE8506058L (en) 1985-12-20
EP0179862A4 (en) 1988-03-18
KR930011145B1 (en) 1993-11-24
AU4217985A (en) 1985-11-28
BR8506693A (en) 1986-04-15
SE460191B (en) 1989-09-18
GB2176438A (en) 1986-12-31

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