CA1301956C - Method of making an article comprising a tandem groove, and articleproduced by the method - Google Patents
Method of making an article comprising a tandem groove, and articleproduced by the methodInfo
- Publication number
- CA1301956C CA1301956C CA000592332A CA592332A CA1301956C CA 1301956 C CA1301956 C CA 1301956C CA 000592332 A CA000592332 A CA 000592332A CA 592332 A CA592332 A CA 592332A CA 1301956 C CA1301956 C CA 1301956C
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- CA
- Canada
- Prior art keywords
- groove
- feature
- masking layer
- opening
- tandem
- 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 - Lifetime
Links
Classifications
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/26—Optical coupling means
- G02B6/30—Optical coupling means for use between fibre and thin-film device
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/36—Mechanical coupling means
- G02B6/3628—Mechanical coupling means for mounting fibres to supporting carriers
- G02B6/3684—Mechanical coupling means for mounting fibres to supporting carriers characterised by the manufacturing process of surface profiling of the supporting carrier
- G02B6/3692—Mechanical coupling means for mounting fibres to supporting carriers characterised by the manufacturing process of surface profiling of the supporting carrier with surface micromachining involving etching, e.g. wet or dry etching steps
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/36—Mechanical coupling means
- G02B6/38—Mechanical coupling means having fibre to fibre mating means
- G02B6/3801—Permanent connections, i.e. wherein fibres are kept aligned by mechanical means
- G02B6/3803—Adjustment or alignment devices for alignment prior to splicing
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/42—Coupling light guides with opto-electronic elements
- G02B6/4201—Packages, e.g. shape, construction, internal or external details
- G02B6/4202—Packages, e.g. shape, construction, internal or external details for coupling an active element with fibres without intermediate optical elements, e.g. fibres with plane ends, fibres with shaped ends, bundles
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having at least one potential-jump barrier or surface barrier, e.g. PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic System or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/302—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to change their surface-physical characteristics or shape, e.g. etching, polishing, cutting
- H01L21/306—Chemical or electrical treatment, e.g. electrolytic etching
- H01L21/30604—Chemical etching
- H01L21/30608—Anisotropic liquid etching
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/36—Mechanical coupling means
- G02B6/3628—Mechanical coupling means for mounting fibres to supporting carriers
- G02B6/3632—Mechanical coupling means for mounting fibres to supporting carriers characterised by the cross-sectional shape of the mechanical coupling means
- G02B6/3636—Mechanical coupling means for mounting fibres to supporting carriers characterised by the cross-sectional shape of the mechanical coupling means the mechanical coupling means being grooves
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B6/00—Light guides; Structural details of arrangements comprising light guides and other optical elements, e.g. couplings
- G02B6/24—Coupling light guides
- G02B6/36—Mechanical coupling means
- G02B6/3628—Mechanical coupling means for mounting fibres to supporting carriers
- G02B6/3648—Supporting carriers of a microbench type, i.e. with micromachined additional mechanical structures
- G02B6/3652—Supporting carriers of a microbench type, i.e. with micromachined additional mechanical structures the additional structures being prepositioning mounting areas, allowing only movement in one dimension, e.g. grooves, trenches or vias in the microbench surface, i.e. self aligning supporting carriers
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/24—Structurally defined web or sheet [e.g., overall dimension, etc.]
- Y10T428/24479—Structurally defined web or sheet [e.g., overall dimension, etc.] including variation in thickness
Abstract
METHOD OF MAKING AN ARTICLE COMPRISING A TANDEM
GROOVE, AND ARTICLE PRODUCED BY THE METHOD
Abstract Tandem grooves (or other groove-like features) with controlled transition between the narrow and wide portion of the groove can be formed in a semiconductor surface, exemplarily a (100) Si surface, by a method that comprises patterning a first masking layer such that the resulting aperture in the maskinglayer defines the tandem groove, re-covering the narrow part of the aperture with a second masking layer, subjecting the wide portion of the aperture to an initial etch, removing the second masking layer from the narrow part of she aperture, and subjecting the aperture to a further etch such that both the wide and the narrowportions of the tandem groove are completed. The inventive method is advantageously used to produce grooves that allow attachment of a coated opticalfiber to a Si substrate.
GROOVE, AND ARTICLE PRODUCED BY THE METHOD
Abstract Tandem grooves (or other groove-like features) with controlled transition between the narrow and wide portion of the groove can be formed in a semiconductor surface, exemplarily a (100) Si surface, by a method that comprises patterning a first masking layer such that the resulting aperture in the maskinglayer defines the tandem groove, re-covering the narrow part of the aperture with a second masking layer, subjecting the wide portion of the aperture to an initial etch, removing the second masking layer from the narrow part of she aperture, and subjecting the aperture to a further etch such that both the wide and the narrowportions of the tandem groove are completed. The inventive method is advantageously used to produce grooves that allow attachment of a coated opticalfiber to a Si substrate.
Description
13~956 METHOD OF MAKING AN ARTICLE COMPRISING A TANDEM
GROOVE, AND ARTICLE PRODUCED BY THE METHOD
Field of the Invention This application pertains to methods of making articles that comprise S a semiconductor part with a groove therein, the groove adapted for receiving an optical fiber and maintaining the fiber in a predetermined posit.ion.
Back~round of the Invention In the field of optical fiber communications the need for maintaining the end of an optical fiber in fixed position relative to another optical fiber, a 10 planar waveguide, an opto-electronic device, or some other part frequently arises.
Typically the end of the optical fiber is to be maintained in optical coupling relationship with the other part.
A known way of maintaining the end of an optical fiber in a fixed predetermined position comprises providing a semiconductor substrate with a V-15 groove therein, placing the fiber into the V-groove, and maintaining the fiber in the groove by appropriate means. This approach is used, for instance, in an optical fiber connector disclosed in U. S. Patent 3,864,018.
Semiconductor chips cornprising accurately placed, shaped and dimensioned V-grooves can be readily produced by known photolithographic and 20 etching techniques. See, for instance, U. S. Patents 3,765,969 and 3,506,509,which disclose menns for anisotropic etching of Si. See also K. E. Bean, EE
Transactions on Electron I)evices, Vol. ED-25(10), pp. 1185-1193 (October 1978),and K. E. Petersen, Proceedings of the IEE~E, Vol~ 70(5), pp. 420-457 (May 1982).
As is well known, optical fibers typically comprise one or more 25 polymer coatings that protect and strengthen the fiber. Since the thickness of the coating typically is not controlled to the same degree that the thickness and concentricity of the fiber are controlled (as well as for other reasons), the coating is generally stripped from the end portion of the fiber before the fiber is coupled to another fiber or device. A bare fiber is, however, relatively fragile, and care 30 must be taken to insure that the bare fiber end is maintained substantially free of mechanical stress. This problem is alleviated if the serniconductor substrate contains a tandem Y-groove, i.e., a V-groove that can accommodate a short lengthof bare fiber together with a portion of the coated fiber. In such a tandem V-groove the coated fiber portion can be epoxied into (or otherwise affixed to) the 35 large cross-section por~ion of the V-groove, thereby providing strain relief,whereas the bare portion of the fiber is affixed to the small cross-section portion .~
, i3q)~9~6 of the V-groove in the usual manner.
The prior art method of making a tandem V-groove in (100) silicon comprises providing an appropriately patterned masking layer (e.g., SiO2 or silicon nitride) that comprises 5 a corner compensation feature of the type shown in F~G. 1. The method also comprises simultaneously etching both parts of the V-groove. See, for instance, KE. Bean, op. cit. The corner compensation feature serves to limit undercutting in the transition region of the tandem V-groove, such that a relatively controlled transition between the large and small cross-section portions of the tandem groove results.
In FIG. 1 is schematically shown a portion of an article 1 comprising a tandem V-groove in (100) Si substrate 10 produced by the prior art method, wherein numerals 11 and 15 refer to the sloping side walls of the wide (14) and narrow (16) portions of the groove, respectively, 12 refers to the masked portion of the Si surface, and dotted lines 13 indicate the shape of the transition region between 14 and 16. Numerals 17 refer to the corner compensation feature of the masking layer.
The prior art technique has several shortcomings. For instance, the presence of the compensation feature restricts the tlow of etchant which, in turn, may result in asymmetry of the groove. Furthermore, the small cross-section portion of the tandem groove is etched to completion long before etching of the remainder o~ the groove is completed. This may result in undercutting oE the Eormer, with attendant reduction oE dimensional control.
Still further, the "ears" (17) resulting from the compen~ation feature may be in the way of the fiber during placemeslt of the ~lber into the groove, since it may not always be practical to remove the ears by etching or other appropriate procedure. Finally, certain combinations oE
Eeature sizes may be completely unattainable by means of corner compensation.
In view of the advantages that a tandem V-groove can offer, a method of producing such a groove that is not subject to some or all oE the shortcomings of the prior art method would be of interest. This application discloses such a method.
Summar~,r of the Invention In accordance with one aspect of the invention there is provided a method of making an article comprising a semiconductor body having a major surface with at least one groove-like longitudinal ~eature therein, the feature comprising a first and a second part having a relatively large and a relative small cross-section, respectively, the method comprising - a) forming a first maskin~ layer on the major surface, and patterning the first masking layer such that an opening is ~ormed therein, the opening comprising a wide and a narrow portion associated with the first and the second part of the groove-like feature, respectively; b) ~3~5~
2a contacting the major surface region that is exposed in the opening in the first masking layer with an anisotropic etchant such that the groove-like feature is formed; CH~CI~ERIZED
IN TH~T the method further comprises c) covering, subsequent to a) and prior to b), the 5 narrow portion of the opening with a second masking layer while leaving essentially uncovered the wide portion of the opening; contacting the major surace region that is exposed in the wide portion of the opening with the anisotropic etchant and terminating the contact before formation of the first part of the groove-like feature is completed; and removing the second mask~ng layer from the narrow portion of the opening.
The inventive method comprises forming a first masking layer on a major surface of an appropriate semiconductor part and patterning the first masking layer such that an opening exposing the underlying semiconductor is fonned therein. The opening defines the outline of the desired tandem groove (or .~ ' .
, ..
~30~L95~;
other groove-like feature) and thus comprises a relatively wide portion and a relatively narrow portion, the former associated with the relatively large cross-section portion of the groove-like feature and the latter with the relatively narrow cross-section por~ion. The method further comprises forming a second 5 masking layer that re-covers the narrow portion of the opening but leaves the wide portion thereof essentially uncovered. Typically this is done by forming a masking layer that covers all of ~he previously fonned opening and removing the portion of the masking layer that covers the wide portion of the opening.
The first and the second masking layers are chosen such that the 10 second masking layer can be removed wilthout completely removing the first masking layer. For instance, the first could be a relatively thick (> 1 ,um) SiO2 layer and the second relatively thin (< 0.5 ~lm) SiO2 layer, or they could be dissimilar materials (e.g., SiO2 and silicon nitride, respectively). The method ~urthermore comprises contacting the semiconductor surface that is exposed in the 15 wide portion of the opening with an appropriate anisotropic etchant, and terminating the initial etch before the wide portion of the groove is completelyformed.
If the semiconductor is Si, the major surface advantageously is parallel to a (100) crystallographic plane, and the axis of the groove is oriented 20 essentially parallel to a [110] crystallographic direction. An exemplary anisotropic etchant is KOH in water and normal propanol (see ~. E. Bean, op. cit.). As is well known to those skilled in the art, this etchant (AS do other known etchants) has a very slow etch rate for Si (111) planes, and thus produces (in the above-specified geometry) a V-groove having (111) side walls.
After termination of the initial etch the second masking layer is removed from the narrow portion of the apçrture such that the semieonductor material underlying the narrow portion of the opening is also e~posed. Finally, the semiconduc~or underlying the opening in the fiTst masking layer is contactedwith the anisotropic etch and etching continued until both the large and the small 30 cross-section portions of the tandem V-groove are fully formed.
The inventive method ma~es it possible to produce tandem grooves without the use of non-planar lithography, e.g., using conventional single layer or tri-level resists. As will be appreciated by those skilled in the art, this is asignificant advantage.
~3~1~5~
E3tching times typically are not critical and are generally easily determined. For instance, if both the large and small cross-section portions of the tandem groove are to be etched to attain full V-shape, then the partial etch appropriately is terminated when the width of the bottom of the groove is S approximately equal to the width of the narrow portion of the opening in the masking layer.
The inventive method has relatively broad applicability and can in principle be used to forrn tandem groo~es of a variety of cross-sectional shapes in a variety of semiconductors (typically having cubic crystal structure). The 10 currently preferred semiconduc~or material is Si, and ~he currendy preferred cross-section shape of the groove-like feature formed by means OI the inventive method is V-like (including an incomplete V, i.e., a groove with sloping walls but flat bottom). Furthermore, ~he inventive method is not limited to making simple tandem grooves but can be used to make more complicated features that comprise 15 one or more portions that require a longer etching time than another portion of the feature. For instance, the feature can be a groove for locating two opposed optical fibers in couplillg relationship, with the feature comprising a central portion having a relatively small cross section and two end portions, each having a relatively large cross section. Furthermore, the inventive method can, with 20 obvious modifications, be used to produce uncc.nnected anisotropically etchedfeatures in a semiconductor surface, with one or more of the features requiring a longer etching time than the remainder.
Brief Description of the Drawin~s FIG. 1 schematically depicts a prior art tandem groove;
FIG. 2, shows in block diagram form major steps of an exemplary embodiment of the inventive method; and FIGS. 3-5 schematically show an article according to the invention at various stages of manufacture.
Detailed Description of Some Preferred Embodiments FIG. 2 outlines important processing steps in an exemplary embodiment of the invention. The steps comprise folmation of the first masking layer on a major suIfacs of a semiconductor body, patterning of the first masking layer to forrn an aperture therein that defines the groove-like feature that is to be formed in the surface, forming a second masking layer over the narrow part of the 35 aperture (typically by depositing and patterning ~e second masking layer), partially etching the wide part of the aperture, removing the second masking layer ~3~ S~
from the narrow part of the aperture, arld completing etching. It will be understood that the inventive method typically also comprises one or more steps such as placing an optical fiber into the groove and securing it therein, attaching one or more opto-electronic components (radiation sources and/or detectors) to the 5 Si substrate, possibly forming a planar waveguide in or on the substrate, providing means for making electrical contact with the component(s), and encapsulating thepackage. These (and possibly other) steps may be conventional and do no~ requiredetailed description.
FIGS. 3-5 schematically show the relevant portion of an exemplary 10 article according to the invention at various stages of manufacture. As shown in FIG. 3, the aIticle comprises a semiconductor body 30, typically a Si chip having a (001) major surface that is at least paItially covered by an approp-riate first masking layer 31, e.g., a relatively thick SiO2 layer grown by a conventional technique. A relatively thick first masking layer may have several advantages. As 15 already indicated, it permits removal of the second masking layer from the narrow portion of the aperture without exposing other portions of the semiconductor surface. Furthermore, a relatively thick first masking layer may have advantageous dielectric properties (e.g., high dielectric strength), result in a low capacitance structure, or be able to carry an imbedded waveguide.
The first masking layer is patterned by an appropriate conventional technique (c.g., llthography and plasma etching) such that an aperture 32 is formed therein, the aperture baring a portion of the Si surface having the shape of the groove-like feature to be formed in the surface. The aperture comprises a relatively wide portion 33 and a relatively narrow portion 34. The longitudinal 25 axis of the aperture advantageously is oriented in a [110] crystallographic direction. The narrow portion of the aperture is then re-covered with an appropriate second masking layer 35, e.g., a relatively thin SiO2 layer. This can, for instance, be accomplished by deposition of the masking layer, remasking, andremoval of the oxide from 33.
After formation of the protective layer on 34 the substrate is contacted with an appropriate anisotropic etching medium, e.g., KOH in propanol and water.The etchant attacks (11 l)-type planes at a very slow rate. As depicted in FIG. 4, this results in formation of a groove having (111)-type side and end walls (40) and ~42), respectively, together with (0()1) bottom (41). Etching is terminated 35 before the final cross section of the wide portion of the groove is attained.Consequently, at this stage of the process the groove will always have a ~at ~ 3~56 bottom. The appropriate etch time is easily determined by a minor amount ofexperimentation. Exemplarily etching is stopped when the width of ~1 is approximately the same as that of 34.
The initial etching step is followed by removal of the second masking 5 layer 35 from the narrow portion of the feature, e.g., by conventional plasma etching. Anisotropic etching is then resumed and carried to completion.
Exemplarily this implies formation of a complete V-groove as shown in FIG. 5, wherein 50 refers to the sloping (111) side wall of the naIrow portion of the tandem groove. ~lowever, etching need not necessarily be carried this far, and in 10 some cases it may be desired to produce a groove-like feature in which one ormore portions have a V-like cross section with a flat bottom. All of the possible cross-sectional shapes are intended to be encompassed by the term "~-groove".
As indicated schematically in FIG. 5 by means of broken line Sl, a tandem groove produced according to the invention may exhibit a minor amount 15 of undercutting in the transition region between the two portions of the groove, since most known applicable anisotropic etchants tend to attack convex corners defined by (lll)-type planes. In many instancGs the presence of a minor amount of undercutting may actually be advantageous since it facilitates longitudinal insertion of a fiber into the groove.
Althollgh the above-described embodirment of the invention is currently preferred there are other embodiments thnt mny also be used advantageously. For instance, the first masking layer can be of intermediate thiclcness te.g., 500 nm) chosen such that it is possible to remove the second masking layer 35 while still retaining a sufficiently thick first masking layer for 25 the final etching step. Subsequent to the completion of the final etching step the masking layer can be removed and a protective layer of the desired thickness (e.g., 10 ~lm SiO2) can be formed on the major surface, including the groove therein, to, for instance, attain a low capacitance structure. This embodiment of the inventive method ~ypically minimi7es undercutting in the transition region, but may result in 30 s~resses in the groove due to a difference in the thermal expansion coefficients of Si and of the protective SiO2 layer thereon.
In a further exemplary embodiment of the invention, the first masking layer is again relatively thick (e.g., 10 ~m SiO2). The second masking layer comprises corner compensation features such as are shown in FIG. 1 and is 35 relatively thin ~e.g., 101) nm SiO2). Ihe resulting "ears" can be easily removed by conventional etching. This embodiment of the inventive method typically results ~3~5~;
in further reduction of undercutting and does not produce stress build-up in thegroove.
Example: A conventional (001) Si wafer was oxidized by a conventional high pressure steam process to form a uniform SiO2 layer (thicknessS about 10 ~lm) thereon. The SiO2 surface was then covered with a conventional photoresist, the photoresist exposed through a mask, the exposed resist developed/patterned, and the wafer plasma etched to form apertures through the SiO2 to the underlying Si, all in conventional manner. The mask contained multiple replicas of a basic pattem that corresponds to an optical bench chip. The 10 basic pattern contains a double rectangle feature having a 400 llm x 2 mm portion and a 200 ,um x 1 mm portion, resulting in apertures substantially as depicted in FIG. 3. The wafer was then re-oxidized by exposure ~o dry oxygen to form a 100 nm SiO2 layer thereon, coated with conventional tri-level photoresist, exposed through a second mask, patterned, and the thin SiO2 layer removed from the wide 15 portion of the aperture by plasma etching, all in conventlonal mamler. Nex~ the wafer was etched in EDP (ethylenediamine pyrocatechol) until the wide portion ofthe V-groove was approximately 3/4 finished (approximately 6 hours). I~e wafer was then dipped in BOE (7:1 HF to NH3F) for about 90 seconds to remove 100 nm of SiO2, thereby baring the narrow portion of the apertures. Finally, the20 wafer was re-etched in EDP until etching of the narrow portion of the V-groove was complete. At approximately the same time etching of the wide portion was complete, resulting in a wafer with tandem V-grooves thereon. After further processing the wafer was sliced, resulting in a multiplicity of "optical bench"
chips to which opto-electronic components as well as an optical fiber can be 25 attached during further processing.
GROOVE, AND ARTICLE PRODUCED BY THE METHOD
Field of the Invention This application pertains to methods of making articles that comprise S a semiconductor part with a groove therein, the groove adapted for receiving an optical fiber and maintaining the fiber in a predetermined posit.ion.
Back~round of the Invention In the field of optical fiber communications the need for maintaining the end of an optical fiber in fixed position relative to another optical fiber, a 10 planar waveguide, an opto-electronic device, or some other part frequently arises.
Typically the end of the optical fiber is to be maintained in optical coupling relationship with the other part.
A known way of maintaining the end of an optical fiber in a fixed predetermined position comprises providing a semiconductor substrate with a V-15 groove therein, placing the fiber into the V-groove, and maintaining the fiber in the groove by appropriate means. This approach is used, for instance, in an optical fiber connector disclosed in U. S. Patent 3,864,018.
Semiconductor chips cornprising accurately placed, shaped and dimensioned V-grooves can be readily produced by known photolithographic and 20 etching techniques. See, for instance, U. S. Patents 3,765,969 and 3,506,509,which disclose menns for anisotropic etching of Si. See also K. E. Bean, EE
Transactions on Electron I)evices, Vol. ED-25(10), pp. 1185-1193 (October 1978),and K. E. Petersen, Proceedings of the IEE~E, Vol~ 70(5), pp. 420-457 (May 1982).
As is well known, optical fibers typically comprise one or more 25 polymer coatings that protect and strengthen the fiber. Since the thickness of the coating typically is not controlled to the same degree that the thickness and concentricity of the fiber are controlled (as well as for other reasons), the coating is generally stripped from the end portion of the fiber before the fiber is coupled to another fiber or device. A bare fiber is, however, relatively fragile, and care 30 must be taken to insure that the bare fiber end is maintained substantially free of mechanical stress. This problem is alleviated if the serniconductor substrate contains a tandem Y-groove, i.e., a V-groove that can accommodate a short lengthof bare fiber together with a portion of the coated fiber. In such a tandem V-groove the coated fiber portion can be epoxied into (or otherwise affixed to) the 35 large cross-section por~ion of the V-groove, thereby providing strain relief,whereas the bare portion of the fiber is affixed to the small cross-section portion .~
, i3q)~9~6 of the V-groove in the usual manner.
The prior art method of making a tandem V-groove in (100) silicon comprises providing an appropriately patterned masking layer (e.g., SiO2 or silicon nitride) that comprises 5 a corner compensation feature of the type shown in F~G. 1. The method also comprises simultaneously etching both parts of the V-groove. See, for instance, KE. Bean, op. cit. The corner compensation feature serves to limit undercutting in the transition region of the tandem V-groove, such that a relatively controlled transition between the large and small cross-section portions of the tandem groove results.
In FIG. 1 is schematically shown a portion of an article 1 comprising a tandem V-groove in (100) Si substrate 10 produced by the prior art method, wherein numerals 11 and 15 refer to the sloping side walls of the wide (14) and narrow (16) portions of the groove, respectively, 12 refers to the masked portion of the Si surface, and dotted lines 13 indicate the shape of the transition region between 14 and 16. Numerals 17 refer to the corner compensation feature of the masking layer.
The prior art technique has several shortcomings. For instance, the presence of the compensation feature restricts the tlow of etchant which, in turn, may result in asymmetry of the groove. Furthermore, the small cross-section portion of the tandem groove is etched to completion long before etching of the remainder o~ the groove is completed. This may result in undercutting oE the Eormer, with attendant reduction oE dimensional control.
Still further, the "ears" (17) resulting from the compen~ation feature may be in the way of the fiber during placemeslt of the ~lber into the groove, since it may not always be practical to remove the ears by etching or other appropriate procedure. Finally, certain combinations oE
Eeature sizes may be completely unattainable by means of corner compensation.
In view of the advantages that a tandem V-groove can offer, a method of producing such a groove that is not subject to some or all oE the shortcomings of the prior art method would be of interest. This application discloses such a method.
Summar~,r of the Invention In accordance with one aspect of the invention there is provided a method of making an article comprising a semiconductor body having a major surface with at least one groove-like longitudinal ~eature therein, the feature comprising a first and a second part having a relatively large and a relative small cross-section, respectively, the method comprising - a) forming a first maskin~ layer on the major surface, and patterning the first masking layer such that an opening is ~ormed therein, the opening comprising a wide and a narrow portion associated with the first and the second part of the groove-like feature, respectively; b) ~3~5~
2a contacting the major surface region that is exposed in the opening in the first masking layer with an anisotropic etchant such that the groove-like feature is formed; CH~CI~ERIZED
IN TH~T the method further comprises c) covering, subsequent to a) and prior to b), the 5 narrow portion of the opening with a second masking layer while leaving essentially uncovered the wide portion of the opening; contacting the major surace region that is exposed in the wide portion of the opening with the anisotropic etchant and terminating the contact before formation of the first part of the groove-like feature is completed; and removing the second mask~ng layer from the narrow portion of the opening.
The inventive method comprises forming a first masking layer on a major surface of an appropriate semiconductor part and patterning the first masking layer such that an opening exposing the underlying semiconductor is fonned therein. The opening defines the outline of the desired tandem groove (or .~ ' .
, ..
~30~L95~;
other groove-like feature) and thus comprises a relatively wide portion and a relatively narrow portion, the former associated with the relatively large cross-section portion of the groove-like feature and the latter with the relatively narrow cross-section por~ion. The method further comprises forming a second 5 masking layer that re-covers the narrow portion of the opening but leaves the wide portion thereof essentially uncovered. Typically this is done by forming a masking layer that covers all of ~he previously fonned opening and removing the portion of the masking layer that covers the wide portion of the opening.
The first and the second masking layers are chosen such that the 10 second masking layer can be removed wilthout completely removing the first masking layer. For instance, the first could be a relatively thick (> 1 ,um) SiO2 layer and the second relatively thin (< 0.5 ~lm) SiO2 layer, or they could be dissimilar materials (e.g., SiO2 and silicon nitride, respectively). The method ~urthermore comprises contacting the semiconductor surface that is exposed in the 15 wide portion of the opening with an appropriate anisotropic etchant, and terminating the initial etch before the wide portion of the groove is completelyformed.
If the semiconductor is Si, the major surface advantageously is parallel to a (100) crystallographic plane, and the axis of the groove is oriented 20 essentially parallel to a [110] crystallographic direction. An exemplary anisotropic etchant is KOH in water and normal propanol (see ~. E. Bean, op. cit.). As is well known to those skilled in the art, this etchant (AS do other known etchants) has a very slow etch rate for Si (111) planes, and thus produces (in the above-specified geometry) a V-groove having (111) side walls.
After termination of the initial etch the second masking layer is removed from the narrow portion of the apçrture such that the semieonductor material underlying the narrow portion of the opening is also e~posed. Finally, the semiconduc~or underlying the opening in the fiTst masking layer is contactedwith the anisotropic etch and etching continued until both the large and the small 30 cross-section portions of the tandem V-groove are fully formed.
The inventive method ma~es it possible to produce tandem grooves without the use of non-planar lithography, e.g., using conventional single layer or tri-level resists. As will be appreciated by those skilled in the art, this is asignificant advantage.
~3~1~5~
E3tching times typically are not critical and are generally easily determined. For instance, if both the large and small cross-section portions of the tandem groove are to be etched to attain full V-shape, then the partial etch appropriately is terminated when the width of the bottom of the groove is S approximately equal to the width of the narrow portion of the opening in the masking layer.
The inventive method has relatively broad applicability and can in principle be used to forrn tandem groo~es of a variety of cross-sectional shapes in a variety of semiconductors (typically having cubic crystal structure). The 10 currently preferred semiconduc~or material is Si, and ~he currendy preferred cross-section shape of the groove-like feature formed by means OI the inventive method is V-like (including an incomplete V, i.e., a groove with sloping walls but flat bottom). Furthermore, ~he inventive method is not limited to making simple tandem grooves but can be used to make more complicated features that comprise 15 one or more portions that require a longer etching time than another portion of the feature. For instance, the feature can be a groove for locating two opposed optical fibers in couplillg relationship, with the feature comprising a central portion having a relatively small cross section and two end portions, each having a relatively large cross section. Furthermore, the inventive method can, with 20 obvious modifications, be used to produce uncc.nnected anisotropically etchedfeatures in a semiconductor surface, with one or more of the features requiring a longer etching time than the remainder.
Brief Description of the Drawin~s FIG. 1 schematically depicts a prior art tandem groove;
FIG. 2, shows in block diagram form major steps of an exemplary embodiment of the inventive method; and FIGS. 3-5 schematically show an article according to the invention at various stages of manufacture.
Detailed Description of Some Preferred Embodiments FIG. 2 outlines important processing steps in an exemplary embodiment of the invention. The steps comprise folmation of the first masking layer on a major suIfacs of a semiconductor body, patterning of the first masking layer to forrn an aperture therein that defines the groove-like feature that is to be formed in the surface, forming a second masking layer over the narrow part of the 35 aperture (typically by depositing and patterning ~e second masking layer), partially etching the wide part of the aperture, removing the second masking layer ~3~ S~
from the narrow part of the aperture, arld completing etching. It will be understood that the inventive method typically also comprises one or more steps such as placing an optical fiber into the groove and securing it therein, attaching one or more opto-electronic components (radiation sources and/or detectors) to the 5 Si substrate, possibly forming a planar waveguide in or on the substrate, providing means for making electrical contact with the component(s), and encapsulating thepackage. These (and possibly other) steps may be conventional and do no~ requiredetailed description.
FIGS. 3-5 schematically show the relevant portion of an exemplary 10 article according to the invention at various stages of manufacture. As shown in FIG. 3, the aIticle comprises a semiconductor body 30, typically a Si chip having a (001) major surface that is at least paItially covered by an approp-riate first masking layer 31, e.g., a relatively thick SiO2 layer grown by a conventional technique. A relatively thick first masking layer may have several advantages. As 15 already indicated, it permits removal of the second masking layer from the narrow portion of the aperture without exposing other portions of the semiconductor surface. Furthermore, a relatively thick first masking layer may have advantageous dielectric properties (e.g., high dielectric strength), result in a low capacitance structure, or be able to carry an imbedded waveguide.
The first masking layer is patterned by an appropriate conventional technique (c.g., llthography and plasma etching) such that an aperture 32 is formed therein, the aperture baring a portion of the Si surface having the shape of the groove-like feature to be formed in the surface. The aperture comprises a relatively wide portion 33 and a relatively narrow portion 34. The longitudinal 25 axis of the aperture advantageously is oriented in a [110] crystallographic direction. The narrow portion of the aperture is then re-covered with an appropriate second masking layer 35, e.g., a relatively thin SiO2 layer. This can, for instance, be accomplished by deposition of the masking layer, remasking, andremoval of the oxide from 33.
After formation of the protective layer on 34 the substrate is contacted with an appropriate anisotropic etching medium, e.g., KOH in propanol and water.The etchant attacks (11 l)-type planes at a very slow rate. As depicted in FIG. 4, this results in formation of a groove having (111)-type side and end walls (40) and ~42), respectively, together with (0()1) bottom (41). Etching is terminated 35 before the final cross section of the wide portion of the groove is attained.Consequently, at this stage of the process the groove will always have a ~at ~ 3~56 bottom. The appropriate etch time is easily determined by a minor amount ofexperimentation. Exemplarily etching is stopped when the width of ~1 is approximately the same as that of 34.
The initial etching step is followed by removal of the second masking 5 layer 35 from the narrow portion of the feature, e.g., by conventional plasma etching. Anisotropic etching is then resumed and carried to completion.
Exemplarily this implies formation of a complete V-groove as shown in FIG. 5, wherein 50 refers to the sloping (111) side wall of the naIrow portion of the tandem groove. ~lowever, etching need not necessarily be carried this far, and in 10 some cases it may be desired to produce a groove-like feature in which one ormore portions have a V-like cross section with a flat bottom. All of the possible cross-sectional shapes are intended to be encompassed by the term "~-groove".
As indicated schematically in FIG. 5 by means of broken line Sl, a tandem groove produced according to the invention may exhibit a minor amount 15 of undercutting in the transition region between the two portions of the groove, since most known applicable anisotropic etchants tend to attack convex corners defined by (lll)-type planes. In many instancGs the presence of a minor amount of undercutting may actually be advantageous since it facilitates longitudinal insertion of a fiber into the groove.
Althollgh the above-described embodirment of the invention is currently preferred there are other embodiments thnt mny also be used advantageously. For instance, the first masking layer can be of intermediate thiclcness te.g., 500 nm) chosen such that it is possible to remove the second masking layer 35 while still retaining a sufficiently thick first masking layer for 25 the final etching step. Subsequent to the completion of the final etching step the masking layer can be removed and a protective layer of the desired thickness (e.g., 10 ~lm SiO2) can be formed on the major surface, including the groove therein, to, for instance, attain a low capacitance structure. This embodiment of the inventive method ~ypically minimi7es undercutting in the transition region, but may result in 30 s~resses in the groove due to a difference in the thermal expansion coefficients of Si and of the protective SiO2 layer thereon.
In a further exemplary embodiment of the invention, the first masking layer is again relatively thick (e.g., 10 ~m SiO2). The second masking layer comprises corner compensation features such as are shown in FIG. 1 and is 35 relatively thin ~e.g., 101) nm SiO2). Ihe resulting "ears" can be easily removed by conventional etching. This embodiment of the inventive method typically results ~3~5~;
in further reduction of undercutting and does not produce stress build-up in thegroove.
Example: A conventional (001) Si wafer was oxidized by a conventional high pressure steam process to form a uniform SiO2 layer (thicknessS about 10 ~lm) thereon. The SiO2 surface was then covered with a conventional photoresist, the photoresist exposed through a mask, the exposed resist developed/patterned, and the wafer plasma etched to form apertures through the SiO2 to the underlying Si, all in conventional manner. The mask contained multiple replicas of a basic pattem that corresponds to an optical bench chip. The 10 basic pattern contains a double rectangle feature having a 400 llm x 2 mm portion and a 200 ,um x 1 mm portion, resulting in apertures substantially as depicted in FIG. 3. The wafer was then re-oxidized by exposure ~o dry oxygen to form a 100 nm SiO2 layer thereon, coated with conventional tri-level photoresist, exposed through a second mask, patterned, and the thin SiO2 layer removed from the wide 15 portion of the aperture by plasma etching, all in conventlonal mamler. Nex~ the wafer was etched in EDP (ethylenediamine pyrocatechol) until the wide portion ofthe V-groove was approximately 3/4 finished (approximately 6 hours). I~e wafer was then dipped in BOE (7:1 HF to NH3F) for about 90 seconds to remove 100 nm of SiO2, thereby baring the narrow portion of the apertures. Finally, the20 wafer was re-etched in EDP until etching of the narrow portion of the V-groove was complete. At approximately the same time etching of the wide portion was complete, resulting in a wafer with tandem V-grooves thereon. After further processing the wafer was sliced, resulting in a multiplicity of "optical bench"
chips to which opto-electronic components as well as an optical fiber can be 25 attached during further processing.
Claims (4)
1. A method of making an article comprising a semiconductor body having a major surface with at least one groove like longitudinal feature therein, the feature comprising a first and a second part having a relatively large and a relative small cross-section, respectively, the method comprising a) forming a first masking layer on the major surface, and patterning the first masking layer such that an opening is formed therein, the opening comprising a wide and a narrow portion associated with the first and the second part of the groove-like feature, respectively;
b) contacting the major surface region that is exposed in the opening in the first masking layer with an anisotropic etchant such that the groove-like feature is formed;
CHARACTERIZED IN THAT the method further comprises c) covering, subsequent to a) and prior to b), the narrow portion of the opening with a second masking layer while leaving essentially uncovered the wide portion of the opening; contacting the major surface region that is exposed in the wide portion of the opening with the anisotropic etchant and terminating the contact before formation of the first part of the groove-like feature is completed; and removing the second masking layer from the narrow portion of the opening.
b) contacting the major surface region that is exposed in the opening in the first masking layer with an anisotropic etchant such that the groove-like feature is formed;
CHARACTERIZED IN THAT the method further comprises c) covering, subsequent to a) and prior to b), the narrow portion of the opening with a second masking layer while leaving essentially uncovered the wide portion of the opening; contacting the major surface region that is exposed in the wide portion of the opening with the anisotropic etchant and terminating the contact before formation of the first part of the groove-like feature is completed; and removing the second masking layer from the narrow portion of the opening.
2. Method of claim 1, wherein the semiconductor body is a Si body, wherein the major surface is substantially parallel to a (001) crystallographic plane, and wherein the longitudinal axis of the groove-like feature is substantially parallel to a [110]
crystallographic direction.
crystallographic direction.
3. Method of claim 1 or 2, wherein the groove-like feature is a tandem V-groove adapted for receiving therein an end portion of an optical fiber.
4. Method of claim 1 or 2, wherein the groove-like feature further comprises a third part, the third part also having a relatively large cross-section, the second part connecting the first and third parts, the groove-like feature being a tandem V-groove adapted for receiving therein in opposed position an end portion of each of two optical fibers such that the two optical fibers are optically coupled.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US07/163,685 US4810557A (en) | 1988-03-03 | 1988-03-03 | Method of making an article comprising a tandem groove, and article produced by the method |
| US163,685 | 1988-03-03 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1301956C true CA1301956C (en) | 1992-05-26 |
Family
ID=22591133
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA000592332A Expired - Lifetime CA1301956C (en) | 1988-03-03 | 1989-02-28 | Method of making an article comprising a tandem groove, and articleproduced by the method |
Country Status (7)
| Country | Link |
|---|---|
| US (1) | US4810557A (en) |
| EP (1) | EP0331333B1 (en) |
| JP (1) | JPH07117614B2 (en) |
| KR (1) | KR910005950B1 (en) |
| CA (1) | CA1301956C (en) |
| DE (1) | DE68907079T2 (en) |
| ES (1) | ES2040996T3 (en) |
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| US4997793A (en) * | 1989-11-21 | 1991-03-05 | Eastman Kodak Company | Method of improving cleaving of diode arrays |
| US5053836A (en) * | 1989-11-21 | 1991-10-01 | Eastman Kodak Company | Cleaving of diode arrays with scribing channels |
| US4957592A (en) * | 1989-12-27 | 1990-09-18 | Xerox Corporation | Method of using erodable masks to produce partially etched structures in ODE wafer structures |
| FR2659148B1 (en) * | 1990-03-01 | 1993-04-16 | Commissariat Energie Atomique | METHOD FOR CONNECTING BETWEEN AN OPTICAL FIBER AND AN OPTICAL MICROGUIDE. |
| US5293516A (en) * | 1992-01-28 | 1994-03-08 | International Business Machines Corporation | Multiprobe apparatus |
| US5656507A (en) * | 1992-01-28 | 1997-08-12 | British Telecommunications Public Limited Company | Process for self-aligning circuit components brought into abutment by surface tension of a molten material and bonding under tension |
| US5217568A (en) * | 1992-02-03 | 1993-06-08 | Motorola, Inc. | Silicon etching process using polymeric mask, for example, to form V-groove for an optical fiber coupling |
| GB9203128D0 (en) * | 1992-02-14 | 1992-04-01 | Lucas Ind Plc | Alignment device for optical fibre |
| US5550088A (en) * | 1993-06-02 | 1996-08-27 | Lucent Technologies Inc. | Fabrication process for a self-aligned optical subassembly |
| US5385635A (en) * | 1993-11-01 | 1995-01-31 | Xerox Corporation | Process for fabricating silicon channel structures with variable cross-sectional areas |
| JP3345518B2 (en) * | 1994-09-28 | 2002-11-18 | 株式会社東芝 | Method for manufacturing optical semiconductor module |
| GB2297626A (en) * | 1995-01-27 | 1996-08-07 | Cambridge Consultants | Miniature mounting grooved substrate |
| US5471552A (en) * | 1995-02-22 | 1995-11-28 | Industrial Technology Research Institute | Fabrication of static-alignment fiber-guiding grooves for planar lightwave circuits |
| US5808293A (en) * | 1996-08-28 | 1998-09-15 | Hewlett-Packard Company | Photo detector with an integrated mirror and a method of making the same |
| IT1286385B1 (en) * | 1996-11-19 | 1998-07-08 | Italtel Spa | PROCEDURE FOR CREATING THE COUPLING IN AN OPTOELECTRONIC DEVICE BETWEEN AN OPTICAL FIBER AND A WAVE GUIDE AND DEVICE |
| GB9700150D0 (en) | 1997-01-07 | 1997-02-26 | Cambridge Consultants | Hybrid chip process |
| US5896481A (en) * | 1997-05-30 | 1999-04-20 | The Boeing Company | Optical subassembly with a groove for aligning an optical device with an optical fiber |
| US6296789B1 (en) | 1998-02-20 | 2001-10-02 | Sumitomo Electric Industries, Ltd. | Optical module and a method of fabricating the same |
| US6282351B1 (en) | 1998-02-20 | 2001-08-28 | Sumitomo Electric Industries, Ltd. | Optical module and a method of fabricating the same |
| US6280102B1 (en) | 1998-02-20 | 2001-08-28 | Sumitomo Electric Industries, Ltd. | Optical module product with sealing cap |
| JPH11258467A (en) | 1998-03-16 | 1999-09-24 | Sumitomo Electric Ind Ltd | Lead frame for optical module, manufacture of optical module and optical module |
| JP4019538B2 (en) | 1998-03-16 | 2007-12-12 | 住友電気工業株式会社 | Optical module substrate and optical module |
| US5995688A (en) * | 1998-06-01 | 1999-11-30 | Lucent Technologies, Inc. | Micro-opto-electromechanical devices and method therefor |
| US6265757B1 (en) | 1999-11-09 | 2001-07-24 | Agere Systems Guardian Corp. | Forming attached features on a semiconductor substrate |
| US6811853B1 (en) | 2000-03-06 | 2004-11-02 | Shipley Company, L.L.C. | Single mask lithographic process for patterning multiple types of surface features |
| US6627096B2 (en) | 2000-05-02 | 2003-09-30 | Shipley Company, L.L.C. | Single mask technique for making positive and negative micromachined features on a substrate |
| US20030021572A1 (en) * | 2001-02-07 | 2003-01-30 | Steinberg Dan A. | V-groove with tapered depth and method for making |
| US6885786B2 (en) * | 2001-02-07 | 2005-04-26 | Shipley Company, L.L.C. | Combined wet and dry etching process for micromachining of crystalline materials |
| US6907150B2 (en) * | 2001-02-07 | 2005-06-14 | Shipley Company, L.L.C. | Etching process for micromachining crystalline materials and devices fabricated thereby |
| US6964804B2 (en) * | 2001-02-14 | 2005-11-15 | Shipley Company, L.L.C. | Micromachined structures made by combined wet and dry etching |
| US20020195417A1 (en) * | 2001-04-20 | 2002-12-26 | Steinberg Dan A. | Wet and dry etching process on <110> silicon and resulting structures |
| KR100439088B1 (en) * | 2001-09-14 | 2004-07-05 | 한국과학기술원 | Optical coupling module with self-aligned etched grooves and method for fabricating the same |
| GB0128617D0 (en) * | 2001-11-29 | 2002-01-23 | Denselight Semiconductors Pte | Self-aligned v-groove and deep trench etching of semiconductors |
| GB0201969D0 (en) * | 2002-01-29 | 2002-03-13 | Qinetiq Ltd | Integrated optics devices |
| US6817776B2 (en) * | 2002-11-19 | 2004-11-16 | International Business Machines Corporation | Method of bonding optical fibers and optical fiber assembly |
| TWI254025B (en) | 2003-05-23 | 2006-05-01 | Rohm & Haas Elect Mat | Etching process for micromachining crystalline materials and devices fabricated thereby |
| US7802928B2 (en) * | 2008-01-04 | 2010-09-28 | Honeywell International Inc. | System and method for fiber based resonator coupling |
| JP2010251588A (en) * | 2009-04-17 | 2010-11-04 | Renesas Electronics Corp | Optical transmitter and method of manufacturing the same |
| US10656362B2 (en) | 2018-01-04 | 2020-05-19 | Globalfoundries Singapore Pte. Ltd. | Gamma groove arrays for interconnecting and mounting devices |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR96065E (en) * | 1967-11-01 | 1972-05-19 | Western Electric Co | Precise semiconductor etching process. |
| US3765969A (en) * | 1970-07-13 | 1973-10-16 | Bell Telephone Labor Inc | Precision etching of semiconductors |
| US3864018A (en) * | 1973-10-18 | 1975-02-04 | Bell Telephone Labor Inc | Method and means for splicing arrays of optical fibers |
| CA1193477A (en) * | 1981-02-24 | 1985-09-17 | Tetsuya Yamasaki | Fixing substrate for optical fibers |
| JPS59197137A (en) * | 1983-04-25 | 1984-11-08 | Fujitsu Ltd | Manufacture of semiconductor device |
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1988
- 1988-03-03 US US07/163,685 patent/US4810557A/en not_active Expired - Lifetime
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1989
- 1989-02-22 ES ES198989301712T patent/ES2040996T3/en not_active Expired - Lifetime
- 1989-02-22 DE DE89301712T patent/DE68907079T2/en not_active Expired - Lifetime
- 1989-02-22 EP EP89301712A patent/EP0331333B1/en not_active Expired - Lifetime
- 1989-02-28 CA CA000592332A patent/CA1301956C/en not_active Expired - Lifetime
- 1989-02-28 KR KR8902381A patent/KR910005950B1/en not_active IP Right Cessation
- 1989-03-03 JP JP1050198A patent/JPH07117614B2/en not_active Expired - Lifetime
Also Published As
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|---|---|
| KR890015039A (en) | 1989-10-28 |
| EP0331333B1 (en) | 1993-06-16 |
| KR910005950B1 (en) | 1991-08-09 |
| DE68907079T2 (en) | 1993-10-07 |
| JPH027010A (en) | 1990-01-11 |
| JPH07117614B2 (en) | 1995-12-18 |
| ES2040996T3 (en) | 1993-11-01 |
| EP0331333A3 (en) | 1991-01-16 |
| DE68907079D1 (en) | 1993-07-22 |
| EP0331333A2 (en) | 1989-09-06 |
| US4810557A (en) | 1989-03-07 |
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