EP2866923A1 - Membrane métallique poreuse fabriquée par bombardement d'ions de gaz noble - Google Patents

Membrane métallique poreuse fabriquée par bombardement d'ions de gaz noble

Info

Publication number
EP2866923A1
EP2866923A1 EP13736514.4A EP13736514A EP2866923A1 EP 2866923 A1 EP2866923 A1 EP 2866923A1 EP 13736514 A EP13736514 A EP 13736514A EP 2866923 A1 EP2866923 A1 EP 2866923A1
Authority
EP
European Patent Office
Prior art keywords
membrane
acceleration voltage
metal
noble gas
bombardment
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Withdrawn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
EP13736514.4A
Other languages
German (de)
English (en)
Inventor
Andreas Kolitsch
Anatoli Rogozin
Stephan Brinke-Seiferth
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.)
I3 Membrane GmbH
Helmholtz Zentrum Dresden Rossendorf eV
Original Assignee
I3 Membrane GmbH
Helmholtz Zentrum Dresden Rossendorf eV
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 I3 Membrane GmbH, Helmholtz Zentrum Dresden Rossendorf eV filed Critical I3 Membrane GmbH
Publication of EP2866923A1 publication Critical patent/EP2866923A1/fr
Withdrawn legal-status Critical Current

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
    • 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
    • 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
    • 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
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
    • H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
    • H01M50/409—Separators, membranes or diaphragms characterised by the material
    • H01M50/431—Inorganic material
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M8/00—Fuel cells; Manufacture thereof
    • H01M8/02—Details
    • H01M8/0289—Means for holding the electrolyte
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2323/00—Details relating to membrane preparation
    • B01D2323/35—Use of magnetic or electrical fields
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells

Definitions

  • the present invention relates to a method for producing a porous metal membrane, such a metal membrane, the use of the metal membrane as well as corresponding filter modules.
  • Polymer membranes have long been known. They are manufactured as flat membranes or hollow fiber membranes, have a more or less high porosity.
  • the most commonly used membrane polymers are polysulfones, polyethersulfones, cellulose, polyamides, etc.
  • the membrane structures are divided into symmetrical and asymmetric structures.
  • the manufacturing method of asymmetric membranes is the so-called phase inversion process. In this case, an originally homogeneous polymer solution is subjected to phase separation by changing the temperature or by contacting with a non-solvent in the liquid or vapor phase. The non-solvent is dissolved out after phase separation and formation of a porous structure.
  • the preparation method is described, for example, in US Pat. No.
  • membranes have different sensitivities to chemicals. For example, membranes made of cellulose acetate are sensitive to strong changes in pH, while polysulfone membranes show good resistance to acids and alkalis, but they are often sensitive to free-radical-forming substances such as chlorine compounds or hydrogen peroxide as well as organic solvents.
  • Another method for producing membranes is the bombardment of thin nonporous polymer film with ions.
  • the polymer material is damaged by the ion bombardment and the resulting damage traces can be widened in a subsequent etching process and thus corresponding channel pores are formed. Since such channels naturally have a certain distance from one another due to their funnel-shaped formation, a membrane is produced which has a lower porosity of only 25 to 30% compared to the membranes produced via the phase inversion process.
  • This process for producing porous films is known, for example, from DE 41 03853 A1 and has been used for several decades. Depending on the duration and type of etching, smaller or larger channels are formed.
  • porous metal foils which are less sensitive to the media to be filtered.
  • a method is known from DE 1 01 64214 A1.
  • a known porous polymer film described above is first produced by ion bombardment and subsequently produced by an etching process. On this a thin metal layer is produced, which is so thin that the pores caused by the ions and subsequent etching remain open in the metal layer. Subsequently, the open pores are flowed through in a galvanic deposition process with a galvanically inactive liquid, so that a thicker metal layer is formed, the pores remain open.
  • the polymer layer is then peeled off. It remains the porous metal foil.
  • a similar method using etching methods is known from DE 1 02010001 504A1. In this case, a very thin microporous layer is achieved in which the carrier material of a porous separating layer applied thereto is in turn removed by chemical methods (sacrificial layer).
  • the disadvantage of this type of production of a metal membrane lies in the complexity and in the ultimately very low porosity of the membrane, since this contains only individual holes caused by the ion traces, which moreover do not lie directly next to one another.
  • Another method for producing porous metal foils is the production of pores with laser technology. This process requires no further chemical additives. The pores are drilled by laser, as described for example in DE 1 02007032231 A1.
  • the advantage of this method lies in the fact that neither chemicals used nor complex etching processes must be used for the production. However, this method can not produce pores smaller than 1 / vm because the technology is limited by the wavelength of the laser light. Since most of the major membrane processes used are in the area of nano-, ultrafiltration or microfiltration, a membrane produced by laser drilling can usually serve only as a prefiltration.
  • Ceramic membranes are ultimately produced via various process stages via sintering of the material. Ceramic membranes are characterized by a high stability to pressure and by a high chemical resistance also to organic Fabrics off. Therefore, ceramic membranes are widely used in the chemical industry. The production of ceramic membranes is characterized by the use of numerous chemicals and a complex manufacturing process. Such a method is known from DE 6001 6093 T2. The disadvantage of such membranes is the lack of flexibility and high fragility and a low flow rate. As with conventional polymer membranes, ceramic membranes have a thin release layer located on a backing, resulting in the disadvantages described. With great effort is trying to produce flexible structures by ceramic materials are applied to nonwovens, as described in DE 10208280A1. Here, the binding ability of the ceramic material on the nonwoven plays a significant role and is influenced by further chemical treatments.
  • the task now is to produce a very thin, flexible and durable membrane with a high strength. It should be dispensed with elaborate production steps with sacrifice of supporting layers or by subsequent detachment of an original membrane.
  • the task is also to achieve a pore structure between 1 0 nm and 1 / vm and to be able to configure these as desired and to be independent of the diameter of ion traces and their etching or laser beams.
  • the porosity should be so high that it is clearly superior to the Ion Trace process.
  • a method is used, which is known in outline and modified from the treatment of metal surfaces.
  • Gas ions are shot into a metal surface (eg titanium) and the ions are implanted into the surface. These remain in the material and lead, for example, to an increased oxidation resistance, as in
  • PI3 plasma immersion ion implantation
  • the plasma immersion ion implantation method is now used such that a very thin foil of metal such as aluminum, titanium, gold, but preferably stainless steel with a thickness of up to 20 ⁇ , preferably between 1 ⁇ and 10 ⁇ accelerated by a first acceleration voltage
  • Noble gas ions such as helium, argon, krypton, but preferably helium and / or argon, in particular from both sides, is bombarded.
  • the ion current is chosen so that it comes to a supersaturation in the metal foil. Then, after supersaturation by bubble segregation, pores form, especially under the metal surface.
  • ionic current which can be controlled by concentration and type of gas as well as set temperature, adjusted working pressure, first acceleration voltage and exposure time, smaller or larger pores are formed, which also vary in their distribution depending on the mentioned parameters (temperature, voltage, ion concentration, time, pressure).
  • the process of pore formation depends on the one hand on the concentration of the gas ions as well as on the time and the temperature.
  • bubble segregation is comparable to the Ostwald ripening: smallest bubbles combine into small bubbles, small to medium and medium to large, etc. as a function of time as a function of the temperature.
  • the result here too is always a Gaussian distribution of the pore size.
  • the advantage of such a distribution is the high porosity which is comparable to that of polymer membranes produced via phase separation, although the manufacturing process is quite different.
  • the ion dose is advantageously from 5E 1 6 to 1 E1 8 ions / cm 2 , in particular within a time of up to 1 0 hours, in particular from 1 min to 10 hours.
  • the opening of the pores formed under the metal surface by ion implantation is performed by sputtering the surface by bombardment with noble gas ions at a second accelerating voltage lower than the first accelerating voltage. This is advantageously achieved by lowering the acceleration voltage to a second acceleration voltage, in particular up to an optimum sputtering rate for the respective metal and the corresponding ion (s) and further plasma generation.
  • the pores can be opened outwards or to other pores, and porous passages through the metal foil can be created.
  • the second acceleration voltage for sputtering is usually between 800 and 5000V.
  • the lowering of the acceleration voltage from the first to the second acceleration voltage is advantageously carried out in one stage.
  • the reduction is advantageously carried out without interruption or only with an interruption time of less than 1 min, in particular 10 s, of the bombardment with noble gas ions.
  • the bombardment with the second acceleration voltage is advantageously carried out pulsed, advantageously with the same pulse lengths and pauses as indicated for the bombardment with the first acceleration voltage.
  • a metal foil made of stainless steel is bombarded, for example, between 1 0 minutes and several hours at temperatures up to 650 ° C and a helium ion dose of 5E 1 6 to 1 E1 8 ions / cm 2 .
  • the pore distribution for example, between 0, 1 ⁇ and 0.4 ⁇ be adjusted so fine by the choice of the parameters mentioned that, for example, the metal membrane so prepared for oil-water separation can also be used by hot waters.
  • the advantage of the membrane according to the invention is that the membrane according to the invention is thinner than the membranes known from the prior art and that the temperature resistance is much higher than in the materials used in the prior art.
  • metal foils can be produced with a significantly higher porosity. It may be 50% to 70% or more according to the invention. Due to its properties, a metal membrane produced according to the invention can be used in numerous fields. Because no carrier material is used in contrast to frequently used polymer membranes in the production process, the separating layer itself represents the membrane, which significantly increases the throughput. In this respect, in contrast to the polymer membrane, pleats can accommodate a multiple of area in a module of the same size.
  • the metal membrane has the advantage during Pleatvorgang that this is flexible due to the natural property of metals and therefore no cracks occur at the Pleatstellen. Furthermore, metal is a substance that is itself far more inert and more resistant to temperature than polymers. In addition, metal has excellent tensile strength and a defined toughness. Thus, a metal membrane according to the invention can advantageously be used at high pressure or high temperatures.
  • a membrane according to the invention can be used, for example, for filtering or separating solutions, suspensions, emulsions, foams, aerosols, gas mixtures, smoke, dust, vapors or mists.
  • sterile filters are needed that sterilize water in a defined way. Due to the inert properties of the membrane according to the invention, it is also possible in the field of microfiltration to use solvents such as e.g. Filter alcohol, for example to remove spores defined.
  • the use as a membrane within batteries In the field of microfiltration (average pore size 0, 1 ⁇ to 0.4 ⁇ ) opened up in particular by the small thickness and by the defined temperature resistance of the material used in the membrane according to the invention, the use as a membrane within batteries.
  • the membrane could be used in lithium batteries to separate the anode and cathode as ion conductors.
  • Use in fuel cells would also be advantageous in terms of the durability of the membrane according to the invention.
  • ultrafiltration average pore size between 0.01 ⁇ to 0, 1 ⁇
  • various applications in areas of the separation of macromolecules, virus filtration but also in bioreactors for the defined release of macromolecules call, in the membrane of the invention can be used.
  • the advantage here is the possibility of steam sterilization of the membrane, which is easy due to the material properties.
  • the membranes produced according to the invention can be used, for example, for the separation of salts within the production of antibiotics.
  • the application is conceivable, for example, for decolorization of liquids in the beverage industry.
  • the membrane of the invention is advantageous.
  • the process is carried out in a sealed chamber.
  • the atmosphere in which the PI3 process is performed may advantageously be formed from one or more noble gases.
  • the pressure immediately before the beginning of the PI3 process is advantageously 10 3 - 10 2 Pa. During the process, this advantageously increases to 0, 1 to 20 Pa.
  • the frequency with which the antenna is fed is advantageously 8 to 20 MHz, typically 1 3 to 1 5 MHz, although frequencies of 100 kHz to 2.45 GHz are also possible.
  • the power with which the antenna is fed is advantageously between 100 and 1000 W, in particular between 300 W and 400 W.
  • the first acceleration voltage is advantageously between 10 and 50 kV, in particular between 20 and 40 kV.
  • the pulse duration of the acceleration voltage is advantageously 5 to 50 / vs. Shorter lengths of 5 to 10 / vs are to be preferred.
  • the pulse frequencies advantageously run in the range of 1 00 Hz to 2 kHz.
  • the advantageous number of pulses is between 500,000 and 2,000,000.
  • a certain ion dose is implanted.
  • the dose per pulse is advantageously 1 ⁇ 10 10 ions / cm 2 to 1 ⁇ 10 12 ions / cm 2 , in particular 5 ⁇ 10 10 ions / cm 2 to 5 ⁇ 10 15 ions / cm 2 .
  • the bombardment of the metal foil with the first acceleration voltage is advantageously carried out from both sides of the metal foil, in particular from thicknesses of the metal foil of 10 / vm, in particular 5 / vm, and more.
  • the firing takes place from both sides at the same time or successively, but advantageously from both sides at the same time.
  • the metal foil is provided in particular completely in the plasma and / or the application of the first acceleration voltage takes place from both sides of the metal foil, so that ions are accelerated from both sides onto the metal foil. If the sides are shot at one after the other, the implantation takes place successively in a two-stage process on both sides of the foil.
  • the bombardment with the second acceleration voltage also takes place on both sides, in particular on both sides at the same time.
  • the bilateral bombardment leads to a more even and faster formation of structures according to the invention.
  • the substrate temperature of the metal foil is usually between 100 and 750 ° C during the bombardment with the first acceleration voltage. Higher temperatures also cause a greater penetration depth of the ions, as the influence of solid-state diffusion also comes into play.
  • the substrate temperature can be adjusted and varied for each process. For example, a beam intensity of 10 / vA / cm 2 at a voltage of 50 kV and a power of 0.5 W / cm 2 is sufficient to heat the substrate to 250 ° C.
  • the temperature can be controlled in particular by varying the pulse rate. For higher temperatures, an additional heating of the films is providable.
  • the frequency should not be higher than 1.5 kHz. At a voltage of only 10 kV, frequencies up to 3.5 kHz are preferred.
  • Fig. 1 a scanning electron micrograph of a stainless steel foil with 5 / vm
  • FIG. 2 a scanning electron micrograph of the stainless steel foil from FIG. 1 in the
  • Figure 1 shows a scanning electron micrograph of a stainless steel foil with 5 / vm thickness after double-sided Argonionenimplantation with an ion dose of 1, 5E 1 5 / cm 2 and sputtering by sputtering.
  • An inductively coupled plasma with a frequency of 1.356 MHz was generated via a water-cooled quartz antenna in a vacuum chamber previously filled with argon at 0.5 Pa. The power coupled into the antenna was 400W.
  • As a pulse voltage for the plasma immersion ion implantation 25kV negative with a pulse duration of 10 / vs and a frequency of 2kHz were applied to the metal foil.
  • An ion dose of 1.5E1 5 / cm 2 was implanted.
  • the surface temperature of the stainless steel foil was controlled with an infrared camera. The temperature was 580 ° C. Subsequently, the acceleration voltage was lowered and the film sputtered at an acceleration voltage of 2kV. At the scanning electron micrograph pore sizes of 0.4 vm to 1 / vm were determined and characterized.
  • FIG. 2 shows a scanning electron micrograph of a cross section through the stainless steel foil of FIG. 1.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Sustainable Energy (AREA)
  • Physics & Mathematics (AREA)
  • Optics & Photonics (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

La présente invention concerne un procédé de fabrication d'une membrane métallique poreuse (taille de pores de 10 nm à 1 µm), ainsi qu'une telle membrane métallique et son utilisation, de même que des modules de filtres correspondants. La porosité doit être élevée au point d'être nettement supérieure au procédé utilisant les pistes ioniques. En outre, on doit pouvoir renoncer le plus possible à utiliser des produits chimiques. Le quadrillage mesure 1 à 20 micromètres. Selon l'invention, le procédé d'implantation ionique par immersion plasma est mis en œuvre de façon à bombarder une feuille de métal très mince avec des ions de gaz noble accélérés par une première tension d'accélération, en particulier sur ses deux faces. Le flux d'ions est choisi de manière à créer une sursaturation dans la feuille métallique. En fonction de la sursaturation, des pores se forment alors par ségrégation de bulles, en particulier sous la surface du métal. L'ouverture des pores formés sous la surface du métal par implantation ionique se fait en pulvérisant la surface par bombardement avec des ions de gaz noble accélérés par une seconde tension d'accélération inférieure à la première.
EP13736514.4A 2012-06-29 2013-06-28 Membrane métallique poreuse fabriquée par bombardement d'ions de gaz noble Withdrawn EP2866923A1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102012105770.2A DE102012105770A1 (de) 2012-06-29 2012-06-29 Metallmembran
PCT/EP2013/063670 WO2014001522A1 (fr) 2012-06-29 2013-06-28 Membrane métallique poreuse fabriquée par bombardement d'ions de gaz noble

Publications (1)

Publication Number Publication Date
EP2866923A1 true EP2866923A1 (fr) 2015-05-06

Family

ID=48783205

Family Applications (1)

Application Number Title Priority Date Filing Date
EP13736514.4A Withdrawn EP2866923A1 (fr) 2012-06-29 2013-06-28 Membrane métallique poreuse fabriquée par bombardement d'ions de gaz noble

Country Status (5)

Country Link
US (1) US20150196879A1 (fr)
EP (1) EP2866923A1 (fr)
CN (1) CN104640618A (fr)
DE (1) DE102012105770A1 (fr)
WO (1) WO2014001522A1 (fr)

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US10653824B2 (en) 2012-05-25 2020-05-19 Lockheed Martin Corporation Two-dimensional materials and uses thereof
US20170036911A1 (en) * 2015-08-05 2017-02-09 Lockheed Martin Corporation Perforated sheets of graphene-based material
US10980919B2 (en) 2016-04-14 2021-04-20 Lockheed Martin Corporation Methods for in vivo and in vitro use of graphene and other two-dimensional materials
US9572918B2 (en) 2013-06-21 2017-02-21 Lockheed Martin Corporation Graphene-based filter for isolating a substance from blood
EP3099645A4 (fr) 2014-01-31 2017-09-27 Lockheed Martin Corporation Procédés de formation de structures composites avec un matériau à deux dimensions à l'aide d'une couche de support non-sacrificielle poreuse
CN104857790A (zh) * 2015-04-17 2015-08-26 成都易态科技有限公司 多孔金属箔在室内气体过滤中的应用及结构
WO2017023376A1 (fr) * 2015-08-05 2017-02-09 Lockheed Martin Corporation Feuilles perforables de matériau à base de graphène
AU2016303049A1 (en) 2015-08-06 2018-03-01 Lockheed Martin Corporation Nanoparticle modification and perforation of graphene
CA3020880A1 (fr) 2016-04-14 2017-10-19 Lockheed Martin Corporation Attenuation interfaciale selective des defauts du graphene
CN111063907B (zh) * 2019-11-21 2021-04-23 一汽解放汽车有限公司 一种复合双极板及其制备方法和应用

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Also Published As

Publication number Publication date
WO2014001522A1 (fr) 2014-01-03
US20150196879A1 (en) 2015-07-16
DE102012105770A1 (de) 2014-01-02
CN104640618A (zh) 2015-05-20

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