EP2004090A1 - Procede de traitement d'un materiau presentant des pores nanometriques - Google Patents
Procede de traitement d'un materiau presentant des pores nanometriquesInfo
- Publication number
- EP2004090A1 EP2004090A1 EP07726331A EP07726331A EP2004090A1 EP 2004090 A1 EP2004090 A1 EP 2004090A1 EP 07726331 A EP07726331 A EP 07726331A EP 07726331 A EP07726331 A EP 07726331A EP 2004090 A1 EP2004090 A1 EP 2004090A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- substance
- pores
- nanoscale pores
- nanoscale
- mixture
- 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- Withdrawn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
- 239000011148 porous material Substances 0.000 title claims abstract description 76
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000463 material Substances 0.000 title claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 70
- 239000007943 implant Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 20
- 239000002904 solvent Substances 0.000 claims description 9
- 239000012535 impurity Substances 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 4
- 230000001747 exhibiting effect Effects 0.000 claims description 3
- 239000003814 drug Substances 0.000 claims description 2
- 238000003672 processing method Methods 0.000 claims description 2
- 230000001960 triggered effect Effects 0.000 claims description 2
- 230000000593 degrading effect Effects 0.000 claims 2
- 238000007599 discharging Methods 0.000 claims 1
- 229940079593 drug Drugs 0.000 claims 1
- 230000008569 process Effects 0.000 description 11
- 239000013543 active substance Substances 0.000 description 8
- 230000035515 penetration Effects 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 6
- KRHYYFGTRYWZRS-UHFFFAOYSA-N hydrofluoric acid Substances F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 239000010703 silicon Substances 0.000 description 6
- 239000004094 surface-active agent Substances 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000004480 active ingredient Substances 0.000 description 4
- 239000012876 carrier material Substances 0.000 description 4
- 238000000151 deposition Methods 0.000 description 4
- 238000002048 anodisation reaction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 230000004907 flux Effects 0.000 description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 description 3
- 231100000252 nontoxic Toxicity 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000000560 biocompatible material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000010169 landfilling Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 231100000331 toxic Toxicity 0.000 description 2
- 230000002588 toxic effect Effects 0.000 description 2
- 206010067482 No adverse event Diseases 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 229910021426 porous silicon Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B08—CLEANING
- B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
- B08B7/00—Cleaning by methods not provided for in a single other subclass or a single group in this subclass
- B08B7/0021—Cleaning by methods not provided for in a single other subclass or a single group in this subclass by liquid gases or supercritical fluids
Definitions
- the present invention relates to a method and a device for the treatment of nanoscale pore-containing material according to claims 1 and 11.
- support materials For the treatment, observation, research or even cultivation of living cells, the use of support materials is known, which can be equipped with a variety of agents.
- the landfilling of active ingredients in nanoscale pores of a biocompatible material is known.
- suitable for this porosified silicon is known.
- HF flux acid
- This attacks the silicon in a corresponding anodization process so that pores are formed on the surface of the silicon whose pore size and structure can be determined by varying different anodization parameters.
- active ingredients from such a carrier body which is as uniform as possible and as precisely as possible, the formation of extremely small structured pores whose geometries are in the nanometer range is desired.
- the present invention is therefore based on the object to improve the treatment of nanoscale pores, especially their surfaces.
- the present invention relates to a method for the treatment of nanoscale pore-containing material, in particular of implant material for the treatment of living cells. It is characterized by the fact that the surface tension of a substance or mixture of substances intended for filling the volumes of the nanoscale pores is reduced.
- This procedure is based on the finding that penetration into the smallest pores is thus also possible for fluids which under normal process conditions are unable to penetrate these regions poorly or at all.
- the transfer of the substance or mixture of substances intended for penetration into the nanoscale pores into a supercritical state is particularly advantageous. This causes the substance or mixture used to take on properties that lie between them, the liquids and gases exhibit. In particular, in this case its surface tension can be reduced by powers, with certain substances, it can even be almost completely degraded, so that this substance can penetrate into the smallest structures of a surface depression in this state.
- CO2 is proposed for use of the substance to be converted to a supercritical state.
- CO2 has the advantage that it is non-toxic when in contact with living cells.
- no disadvantageous effects for the further intended use of the carrier material purified therewith can be caused, in particular not on contact with living cells.
- CO2 is a flux-acid (HF) solvent, so that it dissolves in its adhering flux acid due to its complete penetration into the smallest porous wells, removing it from the surface and completely out of the pore can carry.
- HF flux-acid
- CO2 converted in a supercritical state is well suited for the solution of nonpolar molecules.
- SCCO2 supercritical state
- an auxiliary solvent in particular a surfactant, can be added to the substance to be converted into the supercritical state so that a corresponding microemulsion is produced , there Mycelia form, which enclose the polar substance inside.
- the substances which have been released, ie impurities or residues, are led out of a process chamber for carrying out the process and are precipitated in the gaseous state during expansion of the medium and collected by suitable means, such as filters or activated carbon. In this way, the residues released from the pores can be reliably discharged from the process.
- the carrier material can be subjected to, for example, a substance modifying the surface properties of the nanoscale pores and / or a corresponding processing method.
- a substance modifying the surface properties of the nanoscale pores and / or a corresponding processing method is particularly suitable for this purpose.
- O 2 plasma to produce hydroxyl groups on a silicon surface in order to produce a very specific reaction with the pore surface coordinated with a substance to be introduced into the carrier material.
- This is often a silicon surface, since this biocompatible material, for example, after penetration into a body is either harmlessly encapsulated in this, where it can be removed later if necessary, or degraded to harmless silica, which anyway in Body is present.
- SCCO2 is proposed in a particularly preferred manner because of its non-toxic and highly non-polar substances with respect to non-polar substances. After penetration of this carrier medium into the pores, the active substances contained in it can be deposited therein, for example by attachment to the inner pore surfaces.
- polar substances In order to introduce polar substances into the nanoscale pores, the addition of a surfactant to the substance reduced in its surface tension, in turn, according to the cleaning process described above, is preferably proposed.
- polar substances can now be introduced from the outside into the interior of the nanoscale pores in the opposite direction of transport and, if appropriate, be deposited by depositing a chemical and / or physical reaction with the surface of the pore.
- polar substances Especially good for those landfill types are suitable to the above-described treatment methods 0 2 ⁇ plasma acted on pore surfaces.
- Another possibility for the separation of active substances in the interior of nanoscale pores can be realized by influencing the density of the substance or mixture of substances in the supercritical state. For this purpose, for example, by varying the pressure directly on the mass transport or on the
- Solubility of the SCCO2 be acted upon. That is, first under a sufficiently high pressure, the substance to be introduced is dissolved in the SCCO2 and sufficiently long in time Loading transported to the deepest points of the porous structure. After the expiration of the time scheduled for this transport process, reducing the pressure reduces the density of the CO2 so that, due to the reduced solubility, the active substance to be deposited precipitates out of the CO2 and precipitates inside the nanoscale structures. Another way to influence the density of SCCO2 is to vary its temperature.
- a device for the treatment of such nanoscale pore-containing material in particular of implant material for the treatment of living cells, is proposed below.
- This device is characterized in particular by having means for reducing the surface tension of a substance intended for filling the volumes of the nanoscale pores or of a corresponding substance mixture.
- such means may comprise an average pressure increasing and / or decreasing device, such as a high pressure pump, a compressor, or the like.
- Means for influencing the temperature of the substance or mixture of substances to be converted into a supercritical state are also suitable, for example an electric heater.
- this device may include appropriate retention and / or filter means for receiving discharged pollutants, optionally in combination with pressure and / or temperature-changing agents.
- this device may include appropriate retention and / or filter means for receiving discharged pollutants, optionally in combination with pressure and / or temperature-changing agents.
- the device may also be provided with means for introducing a surfactant into the device.
- a surfactant for example, this may be a corresponding memory, a valve and / or a pressure control device, a metering device and optionally further control and / or control units act.
- memory and / or pressure control means may also be provided for the substance whose surface tension is reduced.
- FIG. 1 shows a flow chart for the symbolic representation of individual steps of a method for the treatment of material having nanoscale pores
- Figure 2 is a schematic plan view of a nano-scale pore exhibiting material
- Figure 3 is an enlarged view of a fragmentary view of Figure 2;
- Figure 4 is a schematic representation of a device suitable for carrying out the method.
- the flowchart 1 represents symbolically individual process steps 2 to 5 for carrying out a method for the treatment of nanoscale pore-containing material, in particular of implant material for the treatment of living cells.
- the arrows 6 symbolize the transitions between the individual method steps 2 to 5.
- the arrow 7 symbolizes an optionally to be performed repetition of the method step. 5
- the surface tension of a substance 10 or substance mixture 10 is reduced, which is provided for filling the volume of nanoscale pores 9 of a material 8 (FIGS. 2, 3).
- the surface tension becomes thereby reduced so much that the substance 10 can completely penetrate into the nanoscale pores 9.
- the substance or the mixture of substances 10 is converted into a supercritical state for this purpose.
- CO2 is particularly preferably used which, on the one hand, has no toxic effects with respect to living cells and, on the other hand, has very good dissolving properties with regard to residues or impurities to be removed from the nanoscale pores, for example resulting from the production process.
- deposition residues from anodization processes for producing the nanostructured pores are to be applied here, such as, for example, hydrofluoric acid (HF) or HNO 3 or other diverse solvents which are not compatible with the organism and the like.
- FIG. 2 serves to illustrate this process, as shown in FIG. 2 in the enlarged view.
- a residue 11 or an impurity 11 which originates, for example, from the production process of the nanoscale pore 9, adheres to the enlarged view shown in sectional view.
- the substance 10, preferably SCCO2, which is in the supercritical state, now has such a reduced surface tension that it can easily penetrate into the interior of this pore and dissolve the impurity contained therein and, as a result, discharge it from the pore 9.
- the substance to be converted into a supercritical state can be used in accordance with process step 3 from FIG HiIfsatessmittel, in particular a surfactant are added.
- This binds polar residues so that their polar side points inwards and their non-polar side faces outwards, which in turn allows a residue-free removal from the nanoscale pore.
- a method step 4 corresponding to FIG. 1 can be carried out.
- the material 8 provided as a carrier material for active substances can be exposed to an O 2 plasma for producing hydroxyl groups, for example on a silicon surface.
- an O 2 plasma for producing hydroxyl groups for example on a silicon surface.
- the method step 5 is carried out according to FIG. 1, in which an active substance 13 to be disposed of in the nanoscale pores 9 is added to the substance or substance mixture 10 acting as the carrier medium and to be displaced in the supercritical state.
- an active substance 13 to be disposed of in the nanoscale pores 9 is added to the substance or substance mixture 10 acting as the carrier medium and to be displaced in the supercritical state.
- a chemical and / or physical reaction between the substance 13 to be deposited and the surface 14 of the nanoscale pores 9 can be triggered for the deposition of the substance 13 to be deposited.
- a device 15 for carrying out these method steps is shown schematically in a simplified embodiment as shown in FIG. It comprises, in addition to a pressure chamber 16 for receiving the nanosize pores 9 having material 8 means 17 for reducing the surface tension of a provided for filling the volumes of the nanoscale pores 9 substance 10.
- These means 17 may include a high-pressure pump 18, a heater 19 and optionally further Control and / or regulating units 20 include.
- CO 2 memory 21 and a memory 22 with the material to be deposited 13 are still shown. They are connected via lines 23, 24 and valves 25 and 26 to the unit 17. This in turn is connected via the line 27 with the chamber 16 in connection.
- the monitoring of the entire system can be done for example by the control unit 28.
- the pressure chamber 16 may comprise a heater 19 and optionally further control and / or regulating units 20.
- auxiliary agents (co-solvents) 12 are added to increase the solubility of the active substance 13 in the carrier medium 10.
Landscapes
- Materials For Medical Uses (AREA)
- Micro-Organisms Or Cultivation Processes Thereof (AREA)
- Apparatus Associated With Microorganisms And Enzymes (AREA)
Abstract
La présente invention concerne un procédé de traitement d'un matériau (8) présentant des pores nanométrique (9), notamment d'un matériau pour implantation pour le traitement de cellules vivantes. Le procédé est caractérisé en ce que la tension de surface d'un matériau (10) prévu pour remplir le volume des pores (9) nanométriques est réduite. La présente invention concerne également un dispositif destiné à la réalisation de ce procédé.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE102006015382A DE102006015382A1 (de) | 2006-04-03 | 2006-04-03 | Verfahren zur Behandlung von nanoskalige Poren aufweisendem Material |
| PCT/EP2007/051308 WO2007115849A1 (fr) | 2006-04-03 | 2007-02-12 | Procede de traitement d'un materiau presentant des pores nanometriques |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| EP2004090A1 true EP2004090A1 (fr) | 2008-12-24 |
Family
ID=37896035
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP07726331A Withdrawn EP2004090A1 (fr) | 2006-04-03 | 2007-02-12 | Procede de traitement d'un materiau presentant des pores nanometriques |
Country Status (4)
| Country | Link |
|---|---|
| US (1) | US20100009077A1 (fr) |
| EP (1) | EP2004090A1 (fr) |
| DE (1) | DE102006015382A1 (fr) |
| WO (1) | WO2007115849A1 (fr) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102015222247B4 (de) * | 2015-11-11 | 2017-10-26 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. | Verfahren und Vorrichtung zum Bearbeiten von Kapillarrohren |
Family Cites Families (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7064070B2 (en) | 1998-09-28 | 2006-06-20 | Tokyo Electron Limited | Removal of CMP and post-CMP residue from semiconductors using supercritical carbon dioxide process |
| US6425956B1 (en) * | 2001-01-05 | 2002-07-30 | International Business Machines Corporation | Process for removing chemical mechanical polishing residual slurry |
| US6905556B1 (en) | 2002-07-23 | 2005-06-14 | Novellus Systems, Inc. | Method and apparatus for using surfactants in supercritical fluid processing of wafers |
| US6989358B2 (en) * | 2002-10-31 | 2006-01-24 | Advanced Technology Materials, Inc. | Supercritical carbon dioxide/chemical formulation for removal of photoresists |
| US20040198066A1 (en) * | 2003-03-21 | 2004-10-07 | Applied Materials, Inc. | Using supercritical fluids and/or dense fluids in semiconductor applications |
| US7250374B2 (en) | 2004-06-30 | 2007-07-31 | Tokyo Electron Limited | System and method for processing a substrate using supercritical carbon dioxide processing |
| US7008853B1 (en) * | 2005-02-25 | 2006-03-07 | Infineon Technologies, Ag | Method and system for fabricating free-standing nanostructures |
| US8414908B2 (en) * | 2005-04-28 | 2013-04-09 | The Regents Of The University Of California | Compositions comprising nanostructures for cell, tissue and artificial organ growth, and methods for making and using same |
| US20060254612A1 (en) * | 2005-05-16 | 2006-11-16 | Micron Technology, Inc. | Polar fluid removal from surfaces using supercritical fluids |
-
2006
- 2006-04-03 DE DE102006015382A patent/DE102006015382A1/de not_active Withdrawn
-
2007
- 2007-02-12 US US12/225,504 patent/US20100009077A1/en not_active Abandoned
- 2007-02-12 EP EP07726331A patent/EP2004090A1/fr not_active Withdrawn
- 2007-02-12 WO PCT/EP2007/051308 patent/WO2007115849A1/fr not_active Ceased
Non-Patent Citations (1)
| Title |
|---|
| See references of WO2007115849A1 * |
Also Published As
| Publication number | Publication date |
|---|---|
| US20100009077A1 (en) | 2010-01-14 |
| DE102006015382A1 (de) | 2007-10-04 |
| WO2007115849A1 (fr) | 2007-10-18 |
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Legal Events
| Date | Code | Title | Description |
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| PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
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| 17P | Request for examination filed |
Effective date: 20081103 |
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| AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): DE FR IT |
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| DAX | Request for extension of the european patent (deleted) | ||
| RBV | Designated contracting states (corrected) |
Designated state(s): DE FR IT |
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| 17Q | First examination report despatched |
Effective date: 20110719 |
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| STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE APPLICATION IS DEEMED TO BE WITHDRAWN |
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| 18D | Application deemed to be withdrawn |
Effective date: 20160901 |