EP0834180A2 - Method and apparatus for a surface-mountable device for protection against electrostatic damage to electronic components - Google Patents
Method and apparatus for a surface-mountable device for protection against electrostatic damage to electronic componentsInfo
- Publication number
- EP0834180A2 EP0834180A2 EP96925471A EP96925471A EP0834180A2 EP 0834180 A2 EP0834180 A2 EP 0834180A2 EP 96925471 A EP96925471 A EP 96925471A EP 96925471 A EP96925471 A EP 96925471A EP 0834180 A2 EP0834180 A2 EP 0834180A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- electrodes
- protection device
- mount
- gap
- substrate
- 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.)
- Granted
Links
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/006—Thin film resistors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C17/00—Apparatus or processes specially adapted for manufacturing resistors
- H01C17/06—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base
- H01C17/075—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thin film techniques
- H01C17/08—Apparatus or processes specially adapted for manufacturing resistors adapted for coating resistive material on a base by thin film techniques by vapour deposition
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/1013—Thin film varistors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01C—RESISTORS
- H01C7/00—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material
- H01C7/10—Non-adjustable resistors formed as one or more layers or coatings; Non-adjustable resistors made from powdered conducting material or powdered semi-conducting material with or without insulating material voltage responsive, i.e. varistors
- H01C7/12—Overvoltage protection resistors
Definitions
- the present invention relates gener ⁇ ally to surface-mountable devices (SMDs) for the protection of electrical circuits. More particularly, this invention relates to surface-mountable devices for protection against electrostatic discharge within electrical circuits.
- SMDs surface-mountable devices
- PC Printed circuit
- Examples of such a devices include silicon diodes and metal oxide varistor (MOV) devices.
- MOV metal oxide varistor
- the present invention is a thin film, electrostatic discharge surface mounted device
- ESD/SMD which comprises three material subassemblies.
- the first subassembly includes the substrate carrier.
- the first or substrate-carrier subassembly comprises a carrier base having two electrodes on the top surface which are separated by a gap of controlled width, and wrap-around terminal pads on the side and bottom of the carrier base.
- the second subassembly or voltage variable polymeric material is applied between the two electrodes and effectively bridges gap between the electrodes.
- the third subassembly or cover coat is placed over the polymeric material and electrodes on the top surface of the first or substrate subassembly.
- the third subassembly provides a protective layer which overlies the second subassembly and electrodes, as well as part of the terminal pads connected to the electrodes, so as to provide protection from impacts, oxidation, and other effects, as will be described further below.
- the third subassembly or protective layer is preferably made of a polymeric material, such as polyurethane or polycarbonate.
- the most preferred supporting substrate is an FR-4 epoxy or a polyimide.
- Another aspect of the invention is a thin film, surface-mounted configuration of the ESD/SMD.
- the device comprises electrodes made of a conductive 5 metal.
- the first conductive metal is preferably, but not exclusively, selected from the group including copper, silver, nickel, titanium, aluminum or alloys of these conductive metals.
- the first conductive metal or electrodes may be deposited onto the first first subassembly in many shapes. Photolithographic, mechanical and laser
- processing techniques may be employed to create very small, intricate and complex electrode geometries, as well as creating an appropriate gap width. This capability, when combined with the extremely thin film coatings applied
- PVD physical vapor deposition
- the location of the electrodes at the top of the substrate of the ESD/SMD enables one to use laser processing methods as a high precision secondary operation, in that way
- FIG. 1 is a perspective view of a copper-plated, FR-4 epoxy sheet used to make a subminiature ESD/SMDs in accordance with the 5 present invention.
- FIG. 2 is a cross-sectional view of a portion of the sheet of FIG. 1, and taken along lines 2-2 of FIG. 1.
- FIG. 3 is a perspective view of the
- FIG. 4 is an enlarged, cut-away 15 perspective view of a portion of the routed sheet of FIG. 3, but with a copper plating layer having been reapplied.
- FIG. 5 is a top perspective view of several portions of the flat, upward-facing
- FIG. 6 is a perspective view of the 25 reverse side of FIG. 5, but after the removal of a strip-like portion of copper plating from the replated sheet of FIG. 5.
- FIG. 7 is a perspective view of the top 57 of the strips 26 of FIG. 6, and showing
- FIG. 8 is a view of a single strip 26 after dipping into a copper plating bath and then a nickel plating bath, with the result that addditional copper layer and a nickel layer are deposited onto the terminal-pads portions of the base copper layer.
- FIG. 9 is a perspective view of the strip of FIG. 8, but after immersion into a tin-lead bath to create another layer over the copper and nickel layers of the terminal pads.
- FIG. 10 shows the strip of FIG. 9, depicting the region where the voltage variable polymeric strip will be applied.
- FIG. 11 shows the strip of FIG. 10, but with an added polymeric material 43 into the gap 25 of the strip 26.
- FIG. 12 shows the strip of FIG. 11, but with an added cover coat 56 over the electrodes 21 and polymeric material 43.
- FIG. 13 shows the individual ESD/SMD in accordance with the invention as it is finally made, and after a so-called dicing operation in which a diamond saw is used to cut the strips along parallel planes to form the individual devices.
- FIG. 14 is a front view of the stencil printing machine used to perform the stencil printing step of the ESD/SMD manufacturing process. Detailed Description
- the thin film, circuit device is an subminiature
- overvoltage protection device in a surface mountable configuration for use in printed circuit board or thick film hybrid circuit technology.
- One given name for the device is an electrostatic discharge surface-mounted
- ESD/SMD surface mountable device
- the surface mountable device is designed to protect against electrostatic discharge (ESD) damage to electronic components.
- ESD electrostatic discharge
- the layout and design of the ESD/SMD device is such that it can be
- the protection device of the present 5 invention are designed to replace silicon diodes and MOV technologies which are commonly used for low power protection applications.
- the protection device generally comprises three material subassemblies. As
- the first subassembly generally includes a substrate carier or substrate 13, electrodes 21, and terminal pads 34, 36 for connecting the protection device 60 to the PC board.
- the second subassembly includes the
- the third subassembly includes the cover coat 56.
- the first or substrate carrier subassenmbly comprises a carrier base 13 having two electrodes 21 on the top surface which are
- the second subassembly or voltage variable polymeric material 43 is
- a cover coat 56 is placed over the polymeric material 43 and the electrodes 21 on the top surface 57 of the substrate subassembly, and partially on the top
- the third subassembly provides protection from impacts which may occur during automated assembly, and protection from oxidation and other effects during use.
- the first or 5 substrate subassembly incorporates a carrier base 13 made of a semi-rigid epoxy material. This material exhibits physical properties nearly identical with the standard substrate material used in the printed circuit board
- the first subassembly furthermore
- the 15 includes two metal electrodes 21 which are a part of the pads 34, 36 as one continuous layer or film.
- the pads 34, 36 are made up of several layers, including a base copper layer 44 which also makes up the
- the supplemental copper layer 46 also makes up a second copper layer of
- the base copper layer of the pads and the electrodes are simultaneously deposited by (1) electrochemical processes, such as the plating
- the two metal electrodes, whether one or two layers (or more) thick are separated by a gap 25 of a controlled width W2.
- the substrate subassembly also contains and
- the 20 supports the two (2) terminal pads 34, 36 on the top 57, bottom 58, and sides 59 of the protection device. These bottom 58 and/or sides 59 of the terminal pads 34, 36 serve to attach the device to the board and provide an
- the electrodes 21 and the terminal pads consist of a copper sheet 44 laminated to the case substrate material 13.
- the other layers are deposited, either
- the gap width W2 between the electrodes 21 are defined by photolithographic techniques and through an
- the nature of the photolithographic process allows for very precise control of the width W2 of the separation of the electrode metallization.
- the gap 25 separating the electrodes 21 extends on
- the electrode metallization can be selected from a variety of elemental or alloy materials, i.e. Cu, Ag, Ni, Ti, Al, NiCr, TiN, etc., to obtain coatings which exhibit desired physical, electrical, and
- Photolithography, mechanical, or laser processing techniques are employed for defining the physical dimensions and width of the gap 25 and of the terminal pads 34, 36.
- the voltage variable polymeric material 43 provides the protection from fast 5 transient overvoltage pulses.
- the polymeric material 43 provides for a non-linear electrical response to an overvoltage condition.
- the polymer 43 is a material comprising finely divided particles dispersed
- the polymeric material 43 consists of conductive particles which are uniformly dispersed throughout an insulating binder. This polymer material 43 exhibits a non-linear
- the cover coat 56 subassembly is applied after the metal deposition, pattern definition, and polymer 43 application process, to the top surface of the substrate/polymer
- the cover coat 56 can be comprised of a variety of materials including plastics, conformal coatings, polymers, and epoxies.
- the cover coat 56 also serves as a vehicle for 5 marking the proective devices 60 with the marking being placed between separate layers, or on the surface of the cover coat 56 through an ink transfer process or laser marking.
- This protective device 60 may be made of
- FIGS. 1 and 2 Shown in FIGS. 1 and 2 is a solid sheet 10 of an FR-4 epoxy with copper plating 12.
- the copper plating 12 and the FR-4 epoxy core 13 of this solid sheet 10 may best be seen in FIG. 2.
- FR-4 epoxy sheet 10 is available from Allied Signal Laminate Systems, Hoosick Falls, New York, as Part No. 0200BED130C1/C1GFN0200 C1/C1A2C. Although FR-4 epoxy is a preferred material, other suitable materials include any
- FR-4 epoxy and polyimide are among the class of materials having physical properties that are nearly identical with the standard substrate material used in the PC board industry. As a result, the protective
- the substrate of the protective device 60 of the present invention also provides desired arc-tracking characteristics, and 5 simultaneously exhibits sufficient mechanical flexibility to remain intact when exposed to the rapid release of energy associated with overvoltage.
- the copper plating 12 is etched away from the solid sheet 10 by a conventional etching process.
- the copper is etched away from the substrate by a ferric
- the FR-4 epoxy sheet 10 having this treated, copper-free surface is then routed or punched to create slots 14 along quadrants of the sheet 10, as may be seen in FIG. 3. Dotted 5 lines visually separate these four quadrants in FIG. 3.
- the width W of the slots 14 (FIG. 4) is about 0.0625 inches.
- the length L of each of the slots 14 (FIG. 3) is approximately 5.125.
- the etched and routed or punched sheet 10 shown in FIG. 3 is again plated with copper. This reapplication of copper occurs through the immersion of the etched and routed
- This copper plating step results in the placement of a copper layer having a
- the copper plating 18 resulting from this step covers both (1) the flat, upper surfaces 22 of the sheet 10;
- interstitial regions 16 that define at least a portion of the slots 14. These interstitial regions 16 must be copper- plated because they will ultimately form a portion of the terminal pads 34, 36 of the
- the uniform thickness of the copper plating will depend upon the ultimate needs of the user.
- Patterned panels are a part of, and are evenly spaced across, this clear mask. These patterned panels are made of an UV light-opaque substance, and are of a size and shape
- the pattern 30 will 25 essentially define the shapes and sizes of the electrodes 21 and polymer strip 43.
- a later step defines the remainder of terminal pads 34, 36. It will be appreciated that the width, length and shape of the electrodes 21 and
- one embodiment of the present invention includes having curved corners 19 (not shown) instead of sharp corners
- This step therefore, defines the gap 25 between the electrodes 21, as well as the notches 23 in the electrodes 21.
- Electrode 21 and gap 25 geometries can be employed to configure very small, intricate, and complex electrode 21 and gap 25 geometries.
- the electrode 21 configuration can be conveniently modified to obtain specific electrical
- the gap width W2 can be changed to provide control of triggering and clamping voltages during an overload event.
- the indicated device construction results in a triggering and
- the backside of the sheet is covered with a photoresist material and an otherwise clear
- a rectangular panel is a part of this clear mask.
- the rectangular panels are made of a UV light-opaque substance, and are of a size corresponding to the size of the panel 28 shown in FIG. 6. Essentially, by placing this mask having these panels onto the replated copper sheet 20, several strips of the flat, downward-facing surfaces 28 of the replated copper sheet 20 are effectively shielded from the effects of the UV light.
- the rectangular panels will essentially define the shapes and sizes of the wide terminal pads 34 and 36 and the lower middle portion 28 of the bottom 58 of the strip 26.
- the copper plating from a portion of the bottom 58 of a strip 26 is defined by a photoresist mask. Particularly, the copper plating from the lower, middle portion 28 of the bottom 58 of the strip 26 is removed.
- a perspective view of this section of this replated sheet 20 is shown in FIG. 6.
- the entire replated, photoresis - covered sheet 20, i.e., the top 57, bottom 58, and sides 59 of that sheet 20, is then subjected to UV light.
- the replated sheet 20 is subjected to the UV light for a time sufficient to ensure curing of all of the photoresist that is not covered by the square panels and rectangular strips of the masks. Thereafter, the masks containing these square panels and rectangular strips are removed from the replated sheet 20.
- the photoresist that was formerly below these square panels remains uncured. This uncured photoresist may be washed from the replated sheet 20 using a 5 solvent.
- the cured photoresist on the remainder of the replated sheet 20 provides protection against the next step in the process. Particularly, the cured photoresist
- the replated sheet 20 is then placed in a chemical bath to remove all of the
- the portion of the sheet 20 between adjacent slots 14 is known as a strip
- This strip has a dimension D as shown in FIG. 4 which defines the length of the device. After completion of several of the operations described in this specification, this strip 26 will ultimately be cut into a plurality of pieces, and each of these pieces becomes an 5 ESD/SMD or protective device 60 in accordance with the invention.
- the underside 58 of the strip 26 has regions along its periphery which still include copper
- peripheral regions 34 and 36 of the underside 58 of the strip 26 form portions of the pads. These pads will ultimately serve as the means for securing the entire, finished protective device 58 to the PC board.
- FIG. 7 is a perspective view of the top-side 57 of the strips 26 of FIG. 6. Generally opposite and coinciding with the lower, middle portions 28 of these strips 26 are linear regions 40 on this top-side 38.
- FIG. 7 is to be referred to in connection with the next step in the manufacture of the invention. In this next
- a photoresist polymer is placed along each of the linear regions 40 of the top side 57 of the strips 26. Through the covering of these linear regions 40, photoresist polymer is also placed along the gap 25 and electrodes 21.
- Electrodes 21 are made of a conductive metal, here copper.
- the photoresist is then treated with UV light, resulting in a curing of the photoresist onto linear region 40.
- the entire strip 26 is dipped into an electrolytic copper plating bath and then an
- the polymer 43 can be be applied in a number of ways.
- the polymer 43 can be applied using the stencil printing machine shown in FIG. 14 in a manner similar to the use of the stencil printing described further 5 below.
- the polymer 43 can be applied manually with a tube of the polymer 43. Other automated means for applying the polymer 43 are possible as well.
- the sheet 20 is heat cured to solidify the polymer 43 to obtain strips 26 that look like the strip 26 in FIG. 11.
- the protective device 60 is the placement, across the length of the most of the top 57 of the strip 26, of a protective layer 56 (FIG. 12) .
- This protective layer 56 is the third subassembly of the present protective device
- the protective layer 56 provides protection from oxidation and impacts during attachment to the PC board.
- 25 layer also serves as a means of providing for a surface for pick and place operations which use a vacuum pick-up tool.
- This protective layer 56 helps to control the melting, ionization and arcing
- the protective layer 56 or cover coat material provides desired arc-quenching characteristics, especially important upon interruption of the fusible link 42. 5
- the application of the cover coat 56 is such that it can be performed in a single processing step using a simple fixture to define the shape of the body of the device. This method of manufacture provides for
- the physical location of the electrode gap 25 is not critical, as in a clamping or die mold method.
- the conformal coating may be mixed with a colored dye prior to application to provide for a color-coded voltage rated
- the protective layer 56 may be comprised of a polymer, preferably a polyuretane gel or paste when a stencil printing cover coat application process is
- a polycarbonate adhesive when an injection mold cover coat application process is used.
- a preferred polyurethane is made by Dymax.
- Other similar gels, pastes, and adhesives are suitable for the invention.
- the protective layer 56 may also be comprised of plastics, conformal coatings and epoxies.
- This protective layer 56 is applied to the strips 26 using a stencil printing 5 process which includes the use of a common stencil printing machine shown in FIG. 14. It has been found that stencil printing is faster than some alternative processes for applying the cover coat 56, such as with an injection
- the material is applied to all of the strips 26 in the stencil printing process.
- the fuses can be tested and packaged in a relatively fast automated processs. With the injection filling process it may be difficult to precisely align the protective devices 60 in testing and packaging 5 equipment due to some non-uniform heights and widths of the cover coat 56.
- the stencil printing machine comprises a slidable plate 70, a base 72. a squeegee arm 74, a squeegee 76, and an overlay
- the overlay 78 is mounted on the base 72 and the squeegee 76 is movably mounted on the squeegee arm 74 above the base 72 and overlay 78.
- the plate 70 is slidable underneath the base 72 and overlay 78.
- the overlay 78 has
- the stencil printing process begins by attaching an adhesive tape under the sheet 20.
- the sheet 20, with the adhesive tape are the adhesive tape
- the cover coat now covers the electrodes 21, the gap, 25, and the polymer 5 strip 43 (FIGS. 12 and 13) .
- the squeegee 76 is then raised, and the sheet 20 is unlodged from the overlay 78.
- the openings 80 in the overlay 78 are wide enough so that the protective layer partially overlaps the pads 34, 36, as shown in
- the material used as the cover coat material should have a viscosity in the paste or gel region so that after the material is spread onto the sheet 20, it will flow in a manner which creates a
- cover coat Although a colorless, clear cover coat is aesthetically pleasing, alternative types of cover coats may be used. For example,
- 25 colored, clear or transparent cover coat materials may be used. These colored materials may be simply manufactured by the addition of a dye to a clear cover coat material. Color coding may be accomplished through the use of
- the strips 26 are then ready for a so-called dicing operation, which separates those strips 26 into individual fuses. In this
- a diamond saw or the like is used to cut the strips 26 along parallel planes 61 (FIG. 12) into individual thin film surface- mounted fuses 60 (FIG. 13) .
- the cuts bisect the notches 23 in the electrodes 21.
- the metalization of the electrodes 21 is removed from the notches 23 or notched areas 23. Specifically, it is easier to cut through notched areas 23 without the electrodes.
- the notches 23 in the places where the dicing is to take place alleviates this possible problem and other possible problems. It should be noted that the notches 23 can extend further toward the pads 34, 36, and that the corners 19
Abstract
Description
Claims
Applications Claiming Priority (5)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US474502 | 1983-03-11 | ||
US47450295A | 1995-06-07 | 1995-06-07 | |
US08/474,940 US6023028A (en) | 1994-05-27 | 1995-06-07 | Surface-mountable device having a voltage variable polgmeric material for protection against electrostatic damage to electronic components |
US474940 | 1995-06-07 | ||
PCT/US1996/012217 WO1996041356A2 (en) | 1995-06-07 | 1996-06-06 | Method and apparatus for a surface-mountable device for protection against electrostatic damage to electronic components |
Publications (2)
Publication Number | Publication Date |
---|---|
EP0834180A2 true EP0834180A2 (en) | 1998-04-08 |
EP0834180B1 EP0834180B1 (en) | 2000-05-17 |
Family
ID=27044479
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP96925471A Expired - Lifetime EP0834180B1 (en) | 1995-06-07 | 1996-06-06 | Method and apparatus for a surface-mountable device for protection against electrostatic damage to electronic components |
Country Status (8)
Country | Link |
---|---|
EP (1) | EP0834180B1 (en) |
JP (1) | JPH11507766A (en) |
CN (1) | CN1191623A (en) |
AT (1) | ATE193149T1 (en) |
AU (1) | AU6597296A (en) |
CA (1) | CA2223746A1 (en) |
DE (1) | DE69608440T2 (en) |
WO (1) | WO1996041356A2 (en) |
Families Citing this family (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1212072A (en) * | 1996-01-22 | 1999-03-24 | 保险丝公司 | Surface mountable electrical device comprising PTC element |
US6023403A (en) * | 1996-05-03 | 2000-02-08 | Littlefuse, Inc. | Surface mountable electrical device comprising a PTC and fusible element |
NL1014319C2 (en) | 2000-02-08 | 2001-08-09 | Fci S Hertogenbosch B V | Connector comprising an ESD suppressor. |
US7258819B2 (en) * | 2001-10-11 | 2007-08-21 | Littelfuse, Inc. | Voltage variable substrate material |
US7567416B2 (en) * | 2005-07-21 | 2009-07-28 | Cooper Technologies Company | Transient voltage protection device, material, and manufacturing methods |
US7567415B2 (en) * | 2006-07-11 | 2009-07-28 | Honeywell International Inc. | Separable transient voltage suppression device |
CN101950645A (en) * | 2010-08-27 | 2011-01-19 | 广东风华高新科技股份有限公司 | Chip overvoltage protector and manufacturing method thereof |
US20120307467A1 (en) * | 2011-06-03 | 2012-12-06 | Navarro Luis A | Oxygen-Barrier Packaged Surface Mount Device |
KR20130117397A (en) * | 2012-04-17 | 2013-10-28 | 주식회사 이노칩테크놀로지 | Circuit protection device |
Family Cites Families (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4097834A (en) * | 1976-04-12 | 1978-06-27 | Motorola, Inc. | Non-linear resistors |
FR2513032B1 (en) * | 1981-09-14 | 1985-12-13 | Carreras Michelle | INTEGRATED PROTECTION AGAINST OVERVOLTAGES OF AN ELECTRONIC CIRCUIT, AND ELECTRONIC CIRCUIT PROTECTED BY THIS DEVICE |
US4726991A (en) * | 1986-07-10 | 1988-02-23 | Eos Technologies Inc. | Electrical overstress protection material and process |
US4977357A (en) * | 1988-01-11 | 1990-12-11 | Shrier Karen P | Overvoltage protection device and material |
US5262754A (en) * | 1992-09-23 | 1993-11-16 | Electromer Corporation | Overvoltage protection element |
US5552757A (en) * | 1994-05-27 | 1996-09-03 | Littelfuse, Inc. | Surface-mounted fuse device |
-
1996
- 1996-06-06 AT AT96925471T patent/ATE193149T1/en not_active IP Right Cessation
- 1996-06-06 CA CA002223746A patent/CA2223746A1/en not_active Abandoned
- 1996-06-06 DE DE69608440T patent/DE69608440T2/en not_active Expired - Fee Related
- 1996-06-06 WO PCT/US1996/012217 patent/WO1996041356A2/en not_active Application Discontinuation
- 1996-06-06 EP EP96925471A patent/EP0834180B1/en not_active Expired - Lifetime
- 1996-06-06 JP JP9502323A patent/JPH11507766A/en active Pending
- 1996-06-06 CN CN96195759A patent/CN1191623A/en active Pending
- 1996-06-06 AU AU65972/96A patent/AU6597296A/en not_active Abandoned
Non-Patent Citations (1)
Title |
---|
See references of WO9641356A3 * |
Also Published As
Publication number | Publication date |
---|---|
DE69608440T2 (en) | 2001-01-04 |
JPH11507766A (en) | 1999-07-06 |
MX9709973A (en) | 1998-06-28 |
CN1191623A (en) | 1998-08-26 |
ATE193149T1 (en) | 2000-06-15 |
WO1996041356A2 (en) | 1996-12-19 |
WO1996041356A3 (en) | 1997-01-30 |
AU6597296A (en) | 1996-12-30 |
CA2223746A1 (en) | 1996-12-19 |
DE69608440D1 (en) | 2000-06-21 |
EP0834180B1 (en) | 2000-05-17 |
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