EP2063981A1 - Microtamis pour la filtration de particules dans des applications microfluides, et sa fabrication - Google Patents
Microtamis pour la filtration de particules dans des applications microfluides, et sa fabricationInfo
- Publication number
- EP2063981A1 EP2063981A1 EP07787543A EP07787543A EP2063981A1 EP 2063981 A1 EP2063981 A1 EP 2063981A1 EP 07787543 A EP07787543 A EP 07787543A EP 07787543 A EP07787543 A EP 07787543A EP 2063981 A1 EP2063981 A1 EP 2063981A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- layer
- membrane
- substrate
- macroporous
- etching process
- 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- Withdrawn
Links
Classifications
-
- 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
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/18—Apparatus therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/08—Flat membrane modules
- B01D63/081—Manufacturing thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D63/00—Apparatus in general for separation processes using semi-permeable membranes
- B01D63/08—Flat membrane modules
- B01D63/088—Microfluidic devices comprising semi-permeable flat membranes
-
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2313/00—Details relating to membrane modules or apparatus
- B01D2313/10—Specific supply elements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00824—Ceramic
- B01J2219/00828—Silicon wafers or plates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00835—Comprising catalytically active material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00837—Materials of construction comprising coatings other than catalytically active coatings
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00819—Materials of construction
- B01J2219/00844—Comprising porous material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00905—Separation
- B01J2219/00907—Separation using membranes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00781—Aspects relating to microreactors
- B01J2219/00905—Separation
- B01J2219/00909—Separation using filters
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
- B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
- B01L3/50—Containers for the purpose of retaining a material to be analysed, e.g. test tubes
- B01L3/502—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures
- B01L3/5027—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip
- B01L3/502753—Containers for the purpose of retaining a material to be analysed, e.g. test tubes with fluid transport, e.g. in multi-compartment structures by integrated microfluidic structures, i.e. dimensions of channels and chambers are such that surface tension forces are important, e.g. lab-on-a-chip characterised by bulk separation arrangements on lab-on-a-chip devices, e.g. for filtration or centrifugation
Definitions
- microfluidic applications many microstructured components have already been proposed.
- microsieves for filtering particles have also been described. For example, from US
- 2005/0092676 Al a microfilter known, which consists of a separation layer and a supporting support layer. Both layers may be porous, wherein an inorganic material such as silicon or organic material such as polymer is proposed for the filter membrane. While the actual separation layer is applied as a filter membrane on the upper side of the carrier layer, the back side of the
- Such filters which are open at the bottom, can not readily be integrated into corresponding microfluidic systems, such as the "lab-on-chip” approach.
- membranes of porous silicon are known with a cavern arranged underneath, which are provided for sensory components.
- a membrane sensor unit with a carrier is known, in which the thermocouples are arranged on a silicon membrane.
- the membrane has nano- or mesoporous areas.
- an insulation trough for thermal insulation is provided underneath the membrane, wherein the insulation trough can also be designed as a cavern.
- Nanopores are generally understood to mean pores with average pore diameters of 2-5 nm. Mesopores, however, have average pore diameters of up to 50 nm. Pores with average pore diameters greater than 50 nm are referred to as macropores. These designations also apply in this present document.
- microfilters known hitherto it has features optimized for applications in microfluidics, such as relatively large pore diameters greater than 50 nm, preferably in the ⁇ m range, in particular 1-5 ⁇ m, in a membrane having.
- the macroporous membrane with a cavity located therebelow can be used as an upstream particulate filter in sensitive fluidic systems.
- Figures Ia and Ib a first embodiment of a manufacturing method of a microsieve
- Figures 2a and 2b show a further embodiment of a manufacturing method of a microsieve in the side view.
- a method is proposed by means of a two-stage etching process with a first and a second etching process: a) provision of an at least partially p-doped Si substrate, b) at least partial formation of a layer of n-doped regions on the Si substrate, c) producing a macroporous layer on the Si substrate by a first
- Etching process and d) transferring the macroporous layer through a second, different from the first, etching process into a cantilevered membrane by creating a cavity under the macroporous layer, the second etching process being electropolishing.
- an at least partially p-doped Si substrate 3 is provided.
- the substrate material preferably has a resistivity of p> 1 ⁇ cm.
- a layer 5 of n-doped regions 5 a, 5 b is formed in regions on the Si substrate 3.
- the layer 5 is a mask, more precisely an n-depth mask, and is arranged around the later membrane area.
- One possibility for forming the n-doped regions 5a, 5b is an implantation process. The implantation zone achieved thereby is inert in the further process steps and serves to suspend the later membrane.
- a macroporous layer 10 is produced on the Si substrate 3 by a first etching process, the electrochemical etching in a hydrofluoric acid-containing (HF) electrolyte being provided here as the first etching process.
- HF hydrofluoric acid-containing
- the macroporous layer 10 is produced in a region not protected by the mask, the later filter region 6.
- the final thickness of the macroporous layer 10 is not yet reached in Fig. 1a, i. the figure in Fig. Ia is a snapshot during the first etching process.
- etching methods such as wet chemical etching in potassium hydroxide (KOH) or reactive ion etching (RIE) ⁇ tzkeime, in particular small depressions, provided for pre-structuring of the macropores to be generated.
- KOH potassium hydroxide
- RIE reactive ion etching
- the macroporous layer 10 itself is then, as already mentioned above, produced by electrochemical etching in a hydrofluoric acid (HF) electrolyte.
- HF hydrofluoric acid
- an organic solvent is used as the wetting agent.
- This organic additive allows the adjustment of the HF concentration as well as a targeted influencing of the formation of the macropores in p-doped silicon substrate 3.
- Suitable solvents are, for example, dimethylformamide (DMF), dimethyl sulfoxide (DMSO) or acetonitrile (MeCN).
- DMF dimethylformamide
- DMSO dimethyl sulfoxide
- MeCN acetonitrile
- the formation of the macropores takes place on the previously provided nucleation nuclei.
- an HF concentration in the range of 1 to 20% m (weight percent) is preferably used.
- the final thickness of the macroporous layer 10, which is converted into a self-supporting membrane 15 in a step d), is preferably in the range between 10 and 50 ⁇ m.
- the transfer of the macroporous layer 10 into a cantilevered membrane 15 is achieved by creating a cavity 20 under the layer 10. It is the
- Cavity 20 by a further electrochemical etching step namely generated by an electropolishing.
- This etching step can advantageously be carried out in the same etching medium as for the production of the macroporous layer 10 by a specific increase in the electrical current density.
- mixtures of highly concentrated HF, alcohol and H 2 O are available, preferably with an HF concentration of 20% m or greater.
- etching rates of over 200 nm / s are achieved.
- the depth of the cavity 20, ie the cavern depth can be adjusted within wide ranges.
- cavities 20 or caverns with a depth of a few microns to over 100 microns are possible.
- etching by means of electropolishing is an isotropic process, it must be prevented by a suitable measure that the membrane 15 is simply dissolved out of the substrate 3 in this etching step.
- a suitable measure is the inert n-doped mask as formed in step b).
- a layer 5 of n-doped regions 5a, 5b is again formed on the Si substrate 3 in step b), wherein now first in the
- the n-doped regions 5a, 5b are applied over the entire surface of the Si substrate 3.
- This intermediate state is not shown in the figures.
- a dry layer is formed Etching method used.
- trench openings are defined by means of an additional mask not shown in the figures, typically resist mask. Trench structures that run the entire thickness of the layer 10 are realized via the trench openings. In this trench process, the openings are etched at least until they reach into the substrate 3.
- openings which in this document are also understood as pores and are essential for the subsequent filter function, are defined solely by the trench structuring.
- any torture geometries are possible because the trimmed n-doped filter region 6 is not attacked in the now to be carried out electropolishing.
- the geometric configuration of the openings such as the width of the openings or their distribution in the macroporous layer 10, so it can be controlled controlled. This procedure is particularly suitable for the production of a very thin sieve.
- a cavity 20 is generated under the macroporous layer 10 by means of electropolishing.
- the membrane 15 after its production with a functional layer, not shown in the figures.
- the membrane 15 can be hydrophilized by a slight oxidation.
- a functional layer a reactive layer or a layer with catalytic properties can also be used.
- the sieve then serves - in addition to the filter function - as a microreactor.
- the functional layer can for this example consist of platinum, palladium or nanocrystalline iron.
- nanocrystalline iron As a functional layer, there are interesting applications in the field of neutralization of environmental toxins. Such nanoparticles have been reported to neutralize heavy metals, dioxin, PCBs and a variety of other toxicants. As a result, such in the input area of a lab-on-chip system
- microsieve 1 for use in microfluidics, the finished microsieve 1 comprising: an at least partially p-doped Si substrate 3 with a cutout, a macroporous, n-doped regions 5a, 5b connected to the Si substrate 3 membrane 15, wherein the recess of the Si substrate 3 is arranged to form a cavity 20 directly under the membrane 15.
- the macroporous membrane 15 preferably has pores or openings with a
- the macroporous membrane 15 may have trench structures extending across the entire thickness of the membrane 15. It is also possible that the membrane 15 is provided with a functional layer, in particular a reactive layer and / or a catalytically active layer.
- a functional layer for example, platinum, palladium or nanocrystalline iron is suitable.
- the manufacture of the microsieve 1 comprises a two-stage etching process, wherein the first etching process is not an electropolishing and creates a macroporous layer 10 on the Si substrate 3, while the second etching process is an electropolishing and a
- microsieve 1 described above makes it possible to use it in microfluidic systems, such as in lab-on-chip systems, in particular if samples are to be examined directly and without prior processing. Such is the use of the
- Microsieve 1 suitable for samples especially from (bio) chemical, medical or clinical areas.
Abstract
L'invention concerne un microtamis (1) pour la filtration des particules dans des applications microfluides ainsi qu'un procédé pour sa fabrication. Le microtamis (1) comprend un substrat (3) en Si dont au moins certaines parties sont dopées positivement et doté d'une découpe et une membrane macroporeuse (15) reliée au substrat (3) en Si par des zones (5a, 5b) dopées négativement. La découpe du substrat (3) en Si est disposée directement en dessous de la membrane (15) de manière à former un espace creux (20).
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006041396A DE102006041396A1 (de) | 2006-09-04 | 2006-09-04 | Mikrosieb zur Filterung von Partikeln in Mikrofluidik-Anwendungen und dessen Herstellung |
PCT/EP2007/057275 WO2008028717A1 (fr) | 2006-09-04 | 2007-07-13 | Microtamis pour la filtration de particules dans des applications microfluides, et sa fabrication |
Publications (1)
Publication Number | Publication Date |
---|---|
EP2063981A1 true EP2063981A1 (fr) | 2009-06-03 |
Family
ID=38537799
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP07787543A Withdrawn EP2063981A1 (fr) | 2006-09-04 | 2007-07-13 | Microtamis pour la filtration de particules dans des applications microfluides, et sa fabrication |
Country Status (4)
Country | Link |
---|---|
US (1) | US20100296986A1 (fr) |
EP (1) | EP2063981A1 (fr) |
DE (1) | DE102006041396A1 (fr) |
WO (1) | WO2008028717A1 (fr) |
Families Citing this family (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US8815104B2 (en) | 2008-03-21 | 2014-08-26 | Alliance For Sustainable Energy, Llc | Copper-assisted, anti-reflection etching of silicon surfaces |
US9034216B2 (en) * | 2009-11-11 | 2015-05-19 | Alliance For Sustainable Energy, Llc | Wet-chemical systems and methods for producing black silicon substrates |
US8828765B2 (en) | 2010-06-09 | 2014-09-09 | Alliance For Sustainable Energy, Llc | Forming high efficiency silicon solar cells using density-graded anti-reflection surfaces |
US11251318B2 (en) | 2011-03-08 | 2022-02-15 | Alliance For Sustainable Energy, Llc | Efficient black silicon photovoltaic devices with enhanced blue response |
DE102014207774B4 (de) * | 2014-04-25 | 2015-12-31 | Robert Bosch Gmbh | Verfahren und Vorrichtung zur Aufreinigung von biologischen Molekülen |
DE102014209193B4 (de) * | 2014-05-15 | 2015-12-31 | Robert Bosch Gmbh | Mikrofluidische Vorrichtung zum Nachweisen von Zellen aus einem Fluid, Verfahren zum Betreiben einer solchen Vorrichtung und Verfahren zum Herstellen einer solchen Vorrichtung |
DE102014209188B4 (de) | 2014-05-15 | 2016-01-14 | Robert Bosch Gmbh | Vorrichtung und Verfahren zum Aufbereiten einer biologischen Probe und Analysesystem zum Analysieren einer biologischen Probe |
US11161066B2 (en) | 2018-09-13 | 2021-11-02 | International Business Machines Corporation | Micro-machined filter for magnetic particles |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4100106C1 (fr) * | 1991-01-04 | 1992-05-27 | Robert Bosch Gmbh, 7000 Stuttgart, De |
Family Cites Families (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE19752208A1 (de) | 1997-11-25 | 1999-06-02 | Bosch Gmbh Robert | Thermischer Membransensor und Verfahren zu seiner Herstellung |
DE10030352A1 (de) | 2000-06-21 | 2002-01-10 | Bosch Gmbh Robert | Mikromechanisches Bauelement, insbesondere Sensorelement, mit einer stabilisierten Membran und Verfahren zur Herstellung eines derartigen Bauelements |
DE10046622B4 (de) * | 2000-09-20 | 2010-05-20 | Robert Bosch Gmbh | Verfahren zur Herstellung einer Membransensoreinheit sowie Membransensoreinheit |
DE10138759A1 (de) * | 2001-08-07 | 2003-03-06 | Bosch Gmbh Robert | Verfahren zur Herstellung eines Halbleiterbauelements sowie Halbleiterbauelement, insbesondere Membransensor |
US7282148B2 (en) * | 2003-10-30 | 2007-10-16 | International Business Machines Corporation | Porous silicon composite structure as large filtration array |
-
2006
- 2006-09-04 DE DE102006041396A patent/DE102006041396A1/de not_active Withdrawn
-
2007
- 2007-07-13 US US12/308,303 patent/US20100296986A1/en not_active Abandoned
- 2007-07-13 WO PCT/EP2007/057275 patent/WO2008028717A1/fr active Application Filing
- 2007-07-13 EP EP07787543A patent/EP2063981A1/fr not_active Withdrawn
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
DE4100106C1 (fr) * | 1991-01-04 | 1992-05-27 | Robert Bosch Gmbh, 7000 Stuttgart, De |
Also Published As
Publication number | Publication date |
---|---|
US20100296986A1 (en) | 2010-11-25 |
WO2008028717A1 (fr) | 2008-03-13 |
DE102006041396A1 (de) | 2008-03-06 |
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