EP1233927A1 - Appareil et procede de formation d'une membrane a pores a l'echelle nanometrique - Google Patents

Appareil et procede de formation d'une membrane a pores a l'echelle nanometrique

Info

Publication number
EP1233927A1
EP1233927A1 EP00980528A EP00980528A EP1233927A1 EP 1233927 A1 EP1233927 A1 EP 1233927A1 EP 00980528 A EP00980528 A EP 00980528A EP 00980528 A EP00980528 A EP 00980528A EP 1233927 A1 EP1233927 A1 EP 1233927A1
Authority
EP
European Patent Office
Prior art keywords
layer
base layer
sacrificial
etch stop
membrane
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.)
Withdrawn
Application number
EP00980528A
Other languages
German (de)
English (en)
Other versions
EP1233927A4 (fr
Inventor
Derek Hansford
Mauro Ferrari
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.)
University of California
University of California Berkeley
University of California San Diego UCSD
Original Assignee
University of California
University of California Berkeley
University of California San Diego UCSD
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 University of California, University of California Berkeley, University of California San Diego UCSD filed Critical University of California
Publication of EP1233927A1 publication Critical patent/EP1233927A1/fr
Publication of EP1233927A4 publication Critical patent/EP1233927A4/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
    • B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
    • B81C1/00134—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems comprising flexible or deformable structures
    • B81C1/00158—Diaphragms, membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0053—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes
    • B01D67/0058—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by selective elimination of components, e.g. by leaching
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0053—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes
    • B01D67/006—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods
    • B01D67/0062—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by elimination of segments of the precursor, e.g. nucleation-track membranes, lithography or laser methods by micromachining techniques, e.g. using masking and etching steps, photolithography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0039—Inorganic membrane manufacture
    • B01D67/0072—Inorganic membrane manufacture by deposition from the gaseous phase, e.g. sputtering, CVD, PVD
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/0215—Silicon carbide; Silicon nitride; Silicon oxycarbide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/02—Inorganic material
    • B01D71/022—Metals
    • B01D71/0221—Group 4 or 5 metals
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/02—Details relating to pores or porosity of the membranes
    • B01D2325/0283—Pore size
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/04—Characteristic thickness
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2325/00—Details relating to properties of membranes
    • B01D2325/08—Patterned membranes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/06—Bio-MEMS
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81B—MICROSTRUCTURAL DEVICES OR SYSTEMS, e.g. MICROMECHANICAL DEVICES
    • B81B2201/00—Specific applications of microelectromechanical systems
    • B81B2201/10—Microfilters, e.g. for gas or fluids
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00—Manufacture or treatment of microstructural devices or systems
    • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
    • B81C2201/0102—Surface micromachining
    • B81C2201/0105—Sacrificial layer
    • B81C2201/0109—Sacrificial layers not provided for in B81C2201/0107 - B81C2201/0108
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00—Manufacture or treatment of microstructural devices or systems
    • B81C2201/01—Manufacture or treatment of microstructural devices or systems in or on a substrate
    • B81C2201/0101—Shaping material; Structuring the bulk substrate or layers on the substrate; Film patterning
    • B81C2201/0128—Processes for removing material
    • B81C2201/013—Etching
    • B81C2201/0135—Controlling etch progression
    • B81C2201/014—Controlling etch progression by depositing an etch stop layer, e.g. silicon nitride, silicon oxide, metal
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B81—MICROSTRUCTURAL TECHNOLOGY
    • B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
    • B81C2201/00—Manufacture or treatment of microstructural devices or systems
    • B81C2201/05—Temporary protection of devices or parts of the devices during manufacturing
    • B81C2201/053—Depositing a protective layers

Definitions

  • This invention relates generally to membranes with nanometer scale pores that may be used in filtering applications More particularly, this invention relates to the use of micro fab ⁇ cation processing techniques to form nanometer scale porous membranes
  • the invention includes a filter comprising a membrane of elemental silicon with sub-fifty nanometer pores formed within it.
  • the membrane has a glucose diffusion test result of at least 1 mg/dl and an albumin diffusion test result of at most 0.1 g/dl.
  • the filter has a substrate, a buried sacrificial etch stop layer positioned on the substrate, with the membrane positioned on the buried sacrificial etch stop layer.
  • the buried sacrificial etch stop layer is silicon nitride.
  • the method of the invention includes forming a membrane with nanometer scale pores.
  • a sacrificial etch stop layer is formed on a substrate.
  • a base layer is constructed on the sacrificial etch stop layer.
  • Micrometer scale pores are formed within the base layer.
  • a sacrificial base layer is built on the base layer. The sacrificial base layer is removed from selected regions of the base layer to define nanometer scale pores within the base layer.
  • FIGURE 1 illustrates a substrate with a sacrificial buried layer formed thereon in accordance with an embodiment of the invention.
  • FIGURE 2 illustrates a base layer formed on the sacrificial buried layer of Figure 1.
  • FIGURE 3 illustrates etched micrometer pores formed within a base layer and stopped by a sacrificial buried layer in accordance with the invention.
  • FIGURE 4 illustrates the deposition of a sacrificial base layer in accordance with an embodiment of the invention.
  • FIGURE 5 illustrates anchors formed in the sacrificial base layer utilized in accordance with the invention.
  • FIGURE 6 illustrates a plug layer formed in accordance with an embodiment of the invention.
  • FIGURE 7 illustrates the plug layer after mechanical polishing in accordance with an embodiment of the invention.
  • FIGURE 8 illustrates a protective layer and resultant selective etching utilized in accordance with an embodiment of the invention.
  • FIGURE 9 illustrates a fully released nanometer scale membrane after removal of the protective layers, and selective regions of the sacrificial buried layer.
  • FIGURE 10 illustrates processing steps used to construct the devices of Figures 1-9.
  • FIGURE 11 illustrates a device used to test the membrane of the invention.
  • FIGURE 12 illustrates glucose diffusion through three different nanopore membranes.
  • FIGURE 13 illustrates diffusion of glucose and albumin through micromachined nanopore membranes.
  • FIGURE 14 illustrates glucose diffusion through micromachined membranes incubated in pure glucose and mixed glucose/albumin solutions.
  • FIGURE 15 illustrates diffusion through millipore membranes incubated in pure glucose and mixed glucose/albumin solutions.
  • FIGURE 16 is a table illustrating diffusion of Albumin through various membranes. Like reference numerals refer to corresponding parts throughout the drawings.
  • the present invention relies upon many prior art techniques in forming a membrane with nanometer scale pores. However, the invention also departs from the prior art in several key respects. These departures from the prior art facilitate the formation of pores less than 50 nanometer.
  • the technique of the invention relies upon a buried sacrificial etch stop layer.
  • the buried sacrificial etch stop layer may be silicon nitride.
  • the buried sacrificial etch stop layer operates as an etch stop, and is then removed to expose the nanopores of the invention.
  • a buried sacrificial etch stop layer as an etchant stop during the formation of nanometer scale pores is believed to be novel. While buried etch stop layers are used for structural purposes in the prior art, it is not believed that the prior art shows or suggests the formation of a buried etch stop layer, which operates as an etchant stop during the formation of pores, and which is subsequently etched away to expose pores.
  • the buried sacrificial etch stop layer facilitates three-dimensional control of the pore structure.
  • Prior art techniques endeavored to control pore structure by balancing the etching of two different layers.
  • the buried sacrificial etch stop technique of the invention facilitates the formation of pores less than 50 nanometers. Moreover, these pores can be uniformly formed across the entire wafer.
  • the buried sacrificial etch stop layer of the invention eliminates the prior art use of diffused boron.
  • diffused boron is used as an etch stop it provides an imprecise membrane depth.
  • boron introduces stresses into the completed membrane.
  • the buried sacrificial etch stop layer of the invention provides absolute etching selectivity, as the layer will not be etched at all by the disclosed KOH etchant. In contrast, boron will be minimally etched in the presence of a KOH etchant.
  • the technique of the invention departs from prior art techniques in another important manner. Namely, the technique of the invention relies upon planarization of the outer structural layer to expose the total pore area, instead of the prior art approach of etching entrance holes in the top layer.
  • the first step in the fabrication protocol is to etch a support ridge structure into a substrate. This is accomplished by simply etching a ridge structure prior to the deposition of the etch stop layer.
  • the ridge provides mechanical rigidity to the subsequently formed membrane structure.
  • the buried sacrificial etch stop layer is then deposited on the substrate.
  • a low stress silicon nitride LSN or nitride
  • LPCVD low pressure chemical vapor depositions
  • 0.4 ⁇ m of silicon nitride was used.
  • Figure 1 illustrates a substrate 20 with a sacrificial etch stop layer 22 formed thereon.
  • the base structural layer (base layer) of the membrane is deposited on top of the stop layer 22. Because the stop layer 22 is thin, the structural layer is deposited down into the support ridges formed in the substrate 20. In one embodiment, 5 ⁇ m of polysilicon is used as the base layer.
  • Figure 2 illustrates the base layer 24 positioned on the stop layer 22. Low stress silicon nitride may also be used as the base layer, in which case it operates as its own etch stop layer.
  • the next processing step is to etch holes in the base layer 24 to define the shape of the pores.
  • Prior art masks may be used to define the pores.
  • the holes may be etched through the polysilicon by chlorine plasma, with a thermally grown oxide layer used as a mask.
  • the buried sacrificial etch stop layer 22 acts as an etch stop for the plasma etching of a silicon base layer 24.
  • Figure 3 illustrates the result of this processing.
  • the figure illustrates holes 26 formed in the base layer 24, but terminating in the buried sacrificial etch stop layer 22. At this stage, the holes 26 define micrometer scale pores.
  • Pore sacrificial oxide is subsequently grown on the base layer 24.
  • Figure 4 illustrates a sacrificial oxide 28 positioned on the base layer 24.
  • This sacrificial oxide 28 is also referred to as a nanometer scale sacrificial base layer or sacrificial base layer.
  • This sacrificial base layer 28 is used to define nanometer scale pores.
  • the thickness of the sacrificial base layer 28 determined the pore size in the final membrane, so control of this step is critical to reproducible membranes. This is accomplished by the thermal oxidation of the base layer 24 (e.g., a growth temperature of between 850-950° for approximately one hour with a ten minute anneal). Naturally, many techniques may be used to form a controlled thickness sacrificial base layer. For example, a thermally evaporated tungsten film can be used as a sacrificial base layer for polymer membranes and selectively removed with hydrogen peroxide.
  • the basic requirement of the sacrificial base layer 28 is the ability to control the thickness with high precision across the entire wafer.
  • a plug structural layer is subsequently deposited to file in the holes 26. This step has been implemented by depositing 1.5 ⁇ m of polysilicon.
  • the resultant plug layer 32 is shown in Figure 6.
  • the plug layer 32 is planarzied down to the base layer, leaving the final structure with the plug layer only in the pore hole openings, as shown in Figure 7.
  • the method of planarization depends on the material used as the plug material.
  • For the hard micro- fabrication materials polysilicon and nitride
  • chemical mechanical polishing was used for planarization.
  • the other materials studied were roughly planarized using a plasma etch, with a quick wet chemical smoothing. This technique has the advantage that, assuming it is not etched by the plasma used, the base layer is not affected, but has the disadvantage of the need for controlled etch timing to avoid completely etching the plugs themselves.
  • FIG. 8 illustrates a protective layer(s) 34.
  • the requirements of the protective layer 34 are that it be impervious to the silicon etch (KOH for these studies) and that it be removed without removing the plug 32 or base 24 structural layers.
  • a thin nitride layer is used as the protective layer (nitride is not etched at all by KOH and dissolves slowly in HF).
  • silicone is used as a protective layer, due to the processing temperature necessary for nitride deposition. (835° C).
  • FIG. 8 illustrates the resultant aperture 36 formed in the substrate 20.
  • each hole 26 defines a nanometer scale pore, with the sacrificial base layer 28 providing aperture size control.
  • Figure 10 summarizes the foregoing processing steps.
  • Figure 10 illustrates that the first processing step is to form a buried sacrificial etch stop layer on a substrate (step 50).
  • a base layer is then constructed on the etch stop layer (step 52).
  • Micrometer scale pores are then etched through the base layer to the etch stop layer (step 54).
  • a sacrificial base layer is then deposited on the base layer (step 56).
  • Anchors are then patterned in the sacrificial base layer (step 58).
  • a plug layer is then formed on the base layer (step 60).
  • the plug layer is subsequently planarized (step 62) and polished (step 64).
  • Protective layers are then formed on the base layer and substrate (step 66).
  • the protective layers are then selectively etched to form an aperture in the substrate (step 68).
  • the protective layer, plug layer, and portions of the buried sacrificial etch stop layer are then released (step 70) in the manner described above.
  • a membrane 40 (with 24.5 nanometer pore size +/- 0.9 nm) of the invention was compared with porous alumina (i.e., a WHATMAN ANODISC membrane with a pore size of .02 microns) and a mixed celluose acetate and nitrate membrane (i.e., a MILLIPORE ISOPORE with a pore size of 0.025 microns). All membranes were examined in vitro by measuring relative concentrations of glucose on both sides of the micro fabricated interface over time, using a mini diffusion chamber constructed around the membranes, as shown in Figure 11.
  • Figure 11 illustrates a chamber 80 with a first compartment 82 and a second compartment 84 with fixed volumes of 2 ml. Sampling ports 86 are provided in each compartment. The compartments are at least partially separated by the desired membrane 90. Preferably, the two compartments are sealed with o-rings and are screwed together.
  • Glucose is measured on either side of the membrane 90 using the diffusion chamber by means of a quantitative enzymatic assay (e.g., TRINDER, SIGMA) and colorometric reading via a spectrophotometer.
  • a quantitative enzymatic assay e.g., TRINDER, SIGMA
  • Samples of 0.1 ml were taken from the diffusion chamber and 10 ul of that were added to 3 ml of glucose reagent in a cuvette, and were mixed gently by inversion. Each tube was incubated for 18 minutes at room temperature and then readings were taken at a wavelength of 505 nm.
  • the reagent is linear up to 750 mg/dl.
  • the diffusion chamber itself was attached to a motor for stirring in order to minimize boundary layer effects (diffusion resistance at the liquid/membrane interface).
  • the receptor cell was first filled with phosphate buffer saline for fifteen minutes before the filling of the donor cell.
  • the donor cell was filled with solutions of glucose in phosphate buffer saline in varying concentrations. These tests were carried out at 37°C.
  • the foregoing results illustrate glucose diffusion test results of at least 1 mg/dl in 330 minutes.
  • the membrane has an albumin diffusion test result of at most 0.1 g/dl in 330 minutes.
  • microfabricated silicon membranes were characterized in terms of glucose diffusion, albumin exclusion and stability in biological environments. Results indicated that glucose does indeed diffuse through microfabricated membranes at a rate comparable to commercially available membranes. At the same time, albumin is excluded from passage. In a mixed solution of glucose and albumin, it has been shown that only glucose diffuses through the membranes. Although several membranes, such as those by WHATMAN and MILLIPORE are available for absolute filtration, these membranes do not have all the desired "ideal" membrane properties, such as stability, bio-compatibility, and well-controlled perm-selectivity.
  • the filter technology of the invention alleviates several of the problems associated with current commercially available separation membranes.
  • membranes can be fabricated with sufficient precision to guarantee high pore uniformity in sub-micron dimensions.
  • the thickness of the thermally grown oxide can be controlled to +/- lnm for nominal pore sizes as small as 18nm. This is the size range needed to obtain absolute protein exclusion and glucose diffusion for biosensor applications.
  • this filter technology can bring in the added advantages of stability, minimal protein adsorption through established silicon surface modification techniques, reusability, and sterilizability.
  • the invention has been disclosed in connection with fabricated elemental silicon.
  • the techniques of the invention may also be used in connection with other bio-compatible materials, such as metals (e.g., titanium), ceramics (e.g., silica or silicon nitride), and polymers (e.g., polytetrafluorethylene, polymethylmethacrylate, polystyrenes, and silicones).
  • metals e.g., titanium
  • ceramics e.g., silica or silicon nitride
  • polymers e.g., polytetrafluorethylene, polymethylmethacrylate, polystyrenes, and silicones.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

L"invention concerne un procédé de formation d"une membrane à pores à l"échelle nanométrique, qui consiste à former, sur un substrat, une couche (50) d"arrêt de gravure perdue. Sur cette dernière, on construit une couche de base (52), dans laquelle on forme des pores (54) à l"échelle micrométrique. Sur la couche de base, on construit une couche de base perdue, laquelle est enlevée de zones choisies de la couche de base afin d"y définir des pores à l"échelle nanométrique. La membrane résultante présente des pores de 50 nanomètres au maximum.
EP00980528A 1999-11-17 2000-11-17 Appareil et procede de formation d'une membrane a pores a l'echelle nanometrique Withdrawn EP1233927A4 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
US16604999P 1999-11-17 1999-11-17
US166049P 1999-11-17
PCT/US2000/031749 WO2001036321A1 (fr) 1999-11-17 2000-11-17 Appareil et procede de formation d"une membrane a pores a l"echelle nanometrique

Publications (2)

Publication Number Publication Date
EP1233927A1 true EP1233927A1 (fr) 2002-08-28
EP1233927A4 EP1233927A4 (fr) 2003-01-08

Family

ID=22601590

Family Applications (1)

Application Number Title Priority Date Filing Date
EP00980528A Withdrawn EP1233927A4 (fr) 1999-11-17 2000-11-17 Appareil et procede de formation d'une membrane a pores a l'echelle nanometrique

Country Status (4)

Country Link
EP (1) EP1233927A4 (fr)
JP (1) JP2003514677A (fr)
AU (1) AU1778101A (fr)
WO (1) WO2001036321A1 (fr)

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US5919364A (en) * 1996-06-24 1999-07-06 Regents Of The University Of California Microfabricated filter and shell constructed with a permeable membrane
US5938923A (en) * 1997-04-15 1999-08-17 The Regents Of The University Of California Microfabricated filter and capsule using a substrate sandwich
US6405066B1 (en) * 2000-03-17 2002-06-11 The Regents Of The University Of California Implantable analyte sensor

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EP1233927A4 (fr) 2003-01-08
AU1778101A (en) 2001-05-30
JP2003514677A (ja) 2003-04-22
WO2001036321A9 (fr) 2002-07-04
WO2001036321A1 (fr) 2001-05-25

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