WO2000038823A1 - Fabrication $i(in situ) de microfiltres a membrane - Google Patents

Fabrication $i(in situ) de microfiltres a membrane Download PDF

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Publication number
WO2000038823A1
WO2000038823A1 PCT/CA1999/001242 CA9901242W WO0038823A1 WO 2000038823 A1 WO2000038823 A1 WO 2000038823A1 CA 9901242 W CA9901242 W CA 9901242W WO 0038823 A1 WO0038823 A1 WO 0038823A1
Authority
WO
WIPO (PCT)
Prior art keywords
blank
membrane
embossing
microfilter
web portion
Prior art date
Application number
PCT/CA1999/001242
Other languages
English (en)
Inventor
Ryan S. Raz
Original Assignee
Morphometrix Technologies Inc.
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 Morphometrix Technologies Inc. filed Critical Morphometrix Technologies Inc.
Priority to EP99962020A priority Critical patent/EP1140332A1/fr
Priority to JP2000590767A priority patent/JP2002533236A/ja
Priority to CA002356684A priority patent/CA2356684A1/fr
Priority to AU18529/00A priority patent/AU1852900A/en
Publication of WO2000038823A1 publication Critical patent/WO2000038823A1/fr

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C59/00—Surface shaping of articles, e.g. embossing; Apparatus therefor
    • B29C59/02—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing
    • B29C59/022—Surface shaping of articles, e.g. embossing; Apparatus therefor by mechanical means, e.g. pressing characterised by the disposition or the configuration, e.g. dimensions, of the embossments or the shaping tools therefor
    • 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
    • B01D67/0002—Organic membrane manufacture
    • B01D67/0023—Organic membrane manufacture by inducing porosity into non porous precursor membranes
    • B01D67/0025—Organic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment, e.g. pore-stretching
    • 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
    • B01D67/0055—Inorganic membrane manufacture by inducing porosity into non porous precursor membranes by mechanical treatment
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B26—HAND CUTTING TOOLS; CUTTING; SEVERING
    • B26F—PERFORATING; PUNCHING; CUTTING-OUT; STAMPING-OUT; SEVERING BY MEANS OTHER THAN CUTTING
    • B26F1/00—Perforating; Punching; Cutting-out; Stamping-out; Apparatus therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/24—Use of template or surface directing agents [SDA]
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/34—Use of radiation
    • 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
    • B01D2325/021—Pore shapes
    • B01D2325/0214—Tapered pores
    • 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
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/14—Filters
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
    • B29L2031/00—Other particular articles
    • B29L2031/755—Membranes, diaphragms

Definitions

  • This invention relates to the manufacture of membrane microfilters.
  • 5 Membrane microfilters as opposed to depth filters, function as simple sieves. If a fluid suspension is passed through a membrane microfilter, all objects within that suspension under a certain size (the pore size) are permitted to pass. Everything else is held back and captured on the membrane microfilter's surface.
  • the quality and performance of membrane microfilters are - j O characterized by the pore size distribution, the number of pores in a given area
  • the dominant technology for the production of membrane microfilters is the track-etch technique.
  • a thin polymeric film is exposed to a collimated beam of massive, -J5 energetic nuclei such as U 235 fission fragments. As the nuclei pass through the film, they break the polymer's backbone bonds, leaving a directed trail of defects.
  • the film is placed in a warm caustic bath where the defect trails are preferentially etched against the bulk of the material. The result is a set of microscopic pores whose average size can be controlled by 20 the etch parameters (temperature, concentration, time) and whose surface density is controlled by the length of time the film is left in the particle beam.
  • track-etch technique places numerous restrictions on the 25 materials used, their thickness and composition. They cannot be too thick or the fission fragments will not leave a complete defect trail. Nor can they be conductive or the charge build-up will distort the otherwise collimated beam.
  • the technique is rather difficult to apply in practice, requiring as it does a particle beam source, which may represent a considerable investment.
  • the track-etching takes place under restrictive conditions that make it impractical to process anything other than continuous rolls of polymeric film material.
  • the second stage etching process is difficult (though not impossible) to control and any piece produced in this way must be further processed to remove traces of the harsh chemical used to manufacture the part.
  • the point of collision between the individual particles and the polymeric film cannot, in general, be controlled. As a consequence, the distribution of the defect trails over the surface of the polymer film is random. One consequence is that the arrangement of pores is also random. Another is that there is a high probability of pore overlap if the defect trails are too close together. This can compromise the cut-off point of the membrane microfilter and is only ameliorated by reducing overall porosity (which itself becomes a limitation). If the polymer material used is particularly thick or the etching process is not carefully controlled, the pores produced can take on a tapered character so that they are not square to the membrane surface. In addition, if the particle beam is not well- collimated, the angle of entry of the particles can vary widely with serious consequences for the quality of the microfilter formed.
  • track-etch membrane microfilters often fail to follow their theoretical models of performance.
  • the restrictions inherent in the manufacturing of track-etch membrane microfilters will often translate into application problems for the designer or engineer.
  • the track-etch membrane is manufactured in a separate process and must eventually be mated to some support structure in order to be used. Affixing the track-etch membrane to this support will necessitate the use of glues or thermo-welding process. Placing the membrane on the support structure is not trivial, nor is maintaining a taut, uniformly-stressed surface.
  • the microfilter's composition may be incompatible with the intended use of the completed part.
  • a solution to these problems is found in a three-step manufacturing process involving the creation of a moulded part, the embossing of that part, and the etching of the embossed region for a controlled breakthrough to create an in situ membrane microfilter on the part.
  • a method for manufacturing a membrane microfilter comprising forming a blank having a web portion defining a filter region, embossing one side of the web portion in the filter region with an array of indentations of cross-sections comparable to a desired pore size of the filter, and ablating material from the web portion in the filter region until the indentation forms through pores of the desired pore size.
  • Figures 1 a, 1 b, and 1c show stages in the production of a blank for application of the method of the invention; all views in this and subsequent figures are cross-sectioned unless otherwise stated; Figures 2a, 2b and 2c show successive stages in the embossing of the moulded blank;
  • Figure 3 shows an embossing tool
  • Figure 4 shows deformation occurring when an embossing tool breaks through the blank
  • Figures 5a and 5b show the result of misalignment of a two-part embossing tool
  • Figure 6 shows damage to the embossing tool caused by it contacting a hard surface
  • Figures 7a and 7b illustrate a method of operating the embossing tool
  • Figures 8a and 8b show etching of the blank from the side opposite the tool
  • Figures 9a and 9b show how pore characteristics can be controlled during the etching
  • Figures 10a, 10b and 10c illustrate how different pore size may be formed in the same blank, Figure 10c being a plan view.
  • Figure 1 illustrates the formation of a blank to be subsequently provided with an integral microfilter.
  • the precise technique used to create the moulded blank is not important to the invention.
  • the blank may be pressure moulded from a starting blank c between two mould parts (as in Figure 1 A), together defining a mould cavity d (see Figure 1 B), or may be injection moulded, cast, or manufactured by any other applicable technique.
  • What is important is that the blank has a defined filter region e in which the process membrane microfilter is required. It is usually advisable that this region be relatively thin compared to the rest of the blank, but it should be understood that the final thickness of the filter is determined by subsequent steps of the process. In practice, a thickness much less than 100 microns may be difficult to produce.
  • the filter region c ⁇ where the membrane microfilter is required is embossed (see figure 2), using an embossing tool E having an array of projections g so as to produce an array of indentations in one side of the filter region.
  • the embossing technique is not critical. The embossing may be performed immediately after the blank is moulded while the material is still relatively soft. Alternatively, the embossing may take place as the part is moulded or may be a completely separate step. In any case, the region that requires the microfilter is embossed using a tool having an array of asperities g that can create an array of micro-indentations h in the molded part.
  • the indentations may typically have a diameter up to 10 microns and a separation of at least 10 microns.
  • Embossing tools f whose details include extremely high asperities (see Figure 3) can be easily manufactured by techniques such as microlithography.
  • the drawback to this, or indeed any other embossing tool with such an array of micro-formed features is that the tool must be brought to bear against a hard surface n if the intention is to complete the microfilter formation in this step. If the embossing tool simply breaks through the part to form the microfilter pores, the microfilter itself will be of poor quality, with a deformed surface as seen at k in Figure 4B, with a consequently wide distribution of pore sizes.
  • the embossing tool is designed to break through into a set of aligned wells m, there is a problem in obtaining precise alignment of the asperities with the wells to avoid tool damage (see Figures 5a and 5b). in either case, the tool will rapidly wear out if it is brought to bear against a hard surface during embossing - its delicate microstructure will be destroyed (see figure 6). Instead, the embossing tool is only used to create an array of precisely formed indentations in the microfilter region e of the blank (see Figure 7). It does not
  • the moulded, embossed part e is subjected to an in situ ablation procedure in the region of the embossing (see Figure 8).
  • the ablation procedure may be any one of a range currently available, such as laser ablation, chemical etching, mechanical abrasion, or any other technique that may remove material from a surface in a specified region in a controlled manner. Material may be removed from the side of the region opposite the embossing, or from both sides. As the material is removed from the embossed region, the embossed indentations will reach the opposite surface of the region, forming through pores ⁇ _ in the microfilter region of the blank so that it forms a membrane microfilter.
  • the pore size may be controlled through the etching without comprising porosity or incurring overlap problems.
  • the embossing tool has a microstructure consisting of an array of high-asperity cones then the embossed region will consist of an array of deep, conical wells.
  • a pre-determined cone cross-section is revealed. If the etching is increased, the exposed cross-section is increased and the effective pore size s rises uniformly (see Figure 9).
  • microfilter can be "post-processed" into the filter region of the moulded, embossed part, it is possible to stock-pile an enormous number of blanks for "just-in-time" microfilter manufacture that would correspond to a consumer's requirements. In de-coupling the microfilter blank manufacture from actual microfilter production, both may be separately optimized. This technique then allows the two to be varied independently without compromising the flexibility in pore dimensions often required by a range of customers.
  • the filter region of the blank can be moulded with a minimum thickness of about 100 microns, this being limited by the technique used to form the region, while the area of this region may be as large as required but is typically of the order of one square centimetre or less.
  • any of a number of techniques may be used to produce the surface structure of the embossing tool.
  • the fine structure of that embossing surface depends, to some extent, on the technique used to create it.
  • a presently preferred method for the manufacture of the embossing tool is the LIGA process (X-ray Lithographic, Galvanoformung, Abformtechnik (reference: E.W. Becker et al, Microelectronic Engineering 4, 35-56, 1986).
  • LIGA process X-ray Lithographic, Galvanoformung, Abformtechnik (reference: E.W. Becker et al, Microelectronic Engineering 4, 35-56, 1986).
  • a fine structure can be produced using an X-ray source in a photoresist material.
  • Subsequent development of this resist creates a relief reproduction of the fine structure, although the resist itself is too fragile to be used directly.
  • Electro-deposition fills the resist's surface with metal and when the resist is removed, the metal part is ready
  • a typical embossing tool might have protuberances 10 microns in diameter, spaced by 20 microns.
  • the protuberances themselves may be tapered, as in Figures 7a and 7b, or cylindrical as in Figure 5A.
  • the depth of penetration of the hot embossing tool into the filter region depends on the thickness of the latter but is typically in the range of 10 to 100 microns.
  • a wide range of ablation techniques may be used, of which the following are only exemplary of subtractive micro-machining techniques that may be compatible with the invention having regard to the materials employed.
  • Hot photo-ablation in which material is removed by the action of a laser system (or other light source) that heats, melts and vapourizes the work material to remove it. Again, the action is directional, but the heat-damage effects can make this more difficult to control (a problem that does not appear in the cold- worked process above).
  • Ultrasonic etching in which an ultrasonic tool is set in motion and is coupled to the workpiece by an abrasive slurry. The mechanical motion of the ultrasonic tool drives the abrasive slurry to eat away at the workpiece.
  • Ultra-high precision mechanical machining in which computer numerical controlled (CNC) milling machines capable of 0.05 micron steps are used to remove work material using single crystal diamond tools.
  • CNC computer numerical controlled
  • the quality of the finished filter of the invention should normally be greatly superior to its track-etched counterpart. Pore size can now be controlled to within a narrow tolerance and its statistical distribution is many times narrower than a comparable track-etched membrane.
  • the use of an embossing tool to create the pore distribution over the microfilter's surface means that pore distributing can be precisely controlled.
  • the porosity can be specified to within narrow tolerances depending on the requirements of the application. There is no danger of pore overlap and thus nothing to compromise the integrity of the filter cut-off.
  • embossing tool may be produced with any desired array of cones, which need not all be of the same size (see Figure 10). After the postprocessing etching, these can yield a variety in the size of pores within the filter in any desired arrangement.
  • a great advantage of the process of the invention is that the membrane microfilter can be included in a moulded part without the drawbacks encountered in mechanical mounting methods. This reduces part cost, reduces manufacture time, and eliminates the problem of contamination during the mounting procedure.

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Forests & Forestry (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Filtering Materials (AREA)
  • Shaping Of Tube Ends By Bending Or Straightening (AREA)

Abstract

L'invention concerne la fabrication in situ de microfiltres à membrane, formés dans une région définie d'une ébauche (c) par repoussage d'une surface de ladite région (e) afin d'obtenir un réseau de creux (h), et par ablation du matériau de l'ébauche dans la région définie jusqu'à ce que lesdits creux deviennent des pores traversants (p). L'ablation peut être réalisée par différents moyens tels que l'attaque chimique ou l'ablation au laser.
PCT/CA1999/001242 1998-12-23 1999-12-23 Fabrication $i(in situ) de microfiltres a membrane WO2000038823A1 (fr)

Priority Applications (4)

Application Number Priority Date Filing Date Title
EP99962020A EP1140332A1 (fr) 1998-12-23 1999-12-23 Fabrication in-situ de microfiltres a membrane
JP2000590767A JP2002533236A (ja) 1998-12-23 1999-12-23 薄膜ミクロフィルタの現場での製造
CA002356684A CA2356684A1 (fr) 1998-12-23 1999-12-23 Fabrication (in situ) de microfiltres a membrane
AU18529/00A AU1852900A (en) 1998-12-23 1999-12-23 (in situ) manufacture of membrane microfilters

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US11381498P 1998-12-23 1998-12-23
US60/113,814 1998-12-23

Publications (1)

Publication Number Publication Date
WO2000038823A1 true WO2000038823A1 (fr) 2000-07-06

Family

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Family Applications (1)

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PCT/CA1999/001242 WO2000038823A1 (fr) 1998-12-23 1999-12-23 Fabrication $i(in situ) de microfiltres a membrane

Country Status (5)

Country Link
EP (1) EP1140332A1 (fr)
JP (1) JP2002533236A (fr)
AU (1) AU1852900A (fr)
CA (1) CA2356684A1 (fr)
WO (1) WO2000038823A1 (fr)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003061949A1 (fr) * 2002-01-18 2003-07-31 Avery Dennison Corporation Feuille presentant des structures de l'ordre du micron
WO2004018077A2 (fr) * 2002-08-23 2004-03-04 Daimlerchrysler Ag Corps pour filtre a suie
WO2006057619A1 (fr) * 2004-11-26 2006-06-01 Agency For Science, Technology And Research Procede et appareil pour former des microstructures
NL1028759C2 (nl) * 2005-04-13 2006-10-16 Fluxxion B V Emulsificatie met behulp van microzeef.
US7514045B2 (en) 2002-01-18 2009-04-07 Avery Dennison Corporation Covered microchamber structures
WO2016008586A1 (fr) * 2014-07-18 2016-01-21 Sartorius Stedim Biotech Gmbh Membrane avec cavités macroscopiques multiniveaux à amélioration de performance

Families Citing this family (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7597815B2 (en) * 2003-05-29 2009-10-06 Dressel Pte. Ltd. Process for producing a porous track membrane
PT1704585T (pt) * 2003-12-19 2017-05-05 Univ North Carolina Chapel Hill Métodos para fabricar microestruturas e nanoestruturas isoladas usando litografia suave ou impressão litográfica
WO2006075926A1 (fr) * 2004-12-22 2006-07-20 Dressel Pte. Ltd. Company Carte à membrane et son procédé de fabrication et d'utilisation
TWI506070B (zh) * 2009-12-14 2015-11-01 3M Innovative Properties Co 微穿孔聚合物薄膜及其製造方法與用途
US9266066B2 (en) * 2011-12-13 2016-02-23 Pall Corporation Membrane with localized asymmetries
EP3838385A1 (fr) 2019-12-17 2021-06-23 3M Innovative Properties Company Membranes de polyéthersulfone à surface modifiée par ultrasons et leur procédé de fabrication

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3929135A (en) * 1974-12-20 1975-12-30 Procter & Gamble Absorptive structure having tapered capillaries
US4652412A (en) * 1985-06-14 1987-03-24 Polaroid Corporation Method for forming microporous filter
EP0317399A1 (fr) * 1987-11-13 1989-05-24 Commissariat A L'energie Atomique Membrane microporeuse obtenue par irradiation de deux faces et procédé d'obtention correspondant
US4964992A (en) * 1989-03-21 1990-10-23 Goldsmith Susan H Method of making membrane-type filter and product thereof
EP0648592A2 (fr) * 1993-10-15 1995-04-19 Seiji Kagawa Appareil pour la fabrication d'un film poreux

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3929135A (en) * 1974-12-20 1975-12-30 Procter & Gamble Absorptive structure having tapered capillaries
US4652412A (en) * 1985-06-14 1987-03-24 Polaroid Corporation Method for forming microporous filter
EP0317399A1 (fr) * 1987-11-13 1989-05-24 Commissariat A L'energie Atomique Membrane microporeuse obtenue par irradiation de deux faces et procédé d'obtention correspondant
US4964992A (en) * 1989-03-21 1990-10-23 Goldsmith Susan H Method of making membrane-type filter and product thereof
EP0648592A2 (fr) * 1993-10-15 1995-04-19 Seiji Kagawa Appareil pour la fabrication d'un film poreux

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2003061949A1 (fr) * 2002-01-18 2003-07-31 Avery Dennison Corporation Feuille presentant des structures de l'ordre du micron
US7514045B2 (en) 2002-01-18 2009-04-07 Avery Dennison Corporation Covered microchamber structures
WO2004018077A2 (fr) * 2002-08-23 2004-03-04 Daimlerchrysler Ag Corps pour filtre a suie
WO2004018077A3 (fr) * 2002-08-23 2004-04-22 Daimler Chrysler Ag Corps pour filtre a suie
WO2006057619A1 (fr) * 2004-11-26 2006-06-01 Agency For Science, Technology And Research Procede et appareil pour former des microstructures
NL1028759C2 (nl) * 2005-04-13 2006-10-16 Fluxxion B V Emulsificatie met behulp van microzeef.
WO2006110035A1 (fr) * 2005-04-13 2006-10-19 Fluxxion B.V. Membrane a microtamis pour emulsification et procede lithographique de fabrication afferent
WO2016008586A1 (fr) * 2014-07-18 2016-01-21 Sartorius Stedim Biotech Gmbh Membrane avec cavités macroscopiques multiniveaux à amélioration de performance
US10384168B2 (en) 2014-07-18 2019-08-20 Sartorius Stedim Biotech Gmbh Membrane with performance enhancing multi-level macroscopic cavities

Also Published As

Publication number Publication date
JP2002533236A (ja) 2002-10-08
AU1852900A (en) 2000-07-31
EP1140332A1 (fr) 2001-10-10
CA2356684A1 (fr) 2000-07-06

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