WO2009016419A1 - Probes of enhanced sensitivity for adsorbed molecules detection - Google Patents

Probes of enhanced sensitivity for adsorbed molecules detection Download PDF

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Publication number
WO2009016419A1
WO2009016419A1 PCT/GR2008/000052 GR2008000052W WO2009016419A1 WO 2009016419 A1 WO2009016419 A1 WO 2009016419A1 GR 2008000052 W GR2008000052 W GR 2008000052W WO 2009016419 A1 WO2009016419 A1 WO 2009016419A1
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Prior art keywords
molecules
adsorption
porous
porous medium
metal film
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PCT/GR2008/000052
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French (fr)
Inventor
Alexandros Vradis
Alexandros Koutsioumpas
Nikolaos Spiliopoulos
Dimitrios Anastasopoulos
Georgios Priftis
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University Of Patras
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Publication of WO2009016419A1 publication Critical patent/WO2009016419A1/en

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    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/55—Specular reflectivity
    • G01N21/552—Attenuated total reflection
    • G01N21/553—Attenuated total reflection and using surface plasmons
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/48—Biological material, e.g. blood, urine; Haemocytometers
    • G01N33/50—Chemical analysis of biological material, e.g. blood, urine; Testing involving biospecific ligand binding methods; Immunological testing
    • G01N33/53—Immunoassay; Biospecific binding assay; Materials therefor
    • G01N33/543—Immunoassay; Biospecific binding assay; Materials therefor with an insoluble carrier for immobilising immunochemicals
    • G01N33/54366—Apparatus specially adapted for solid-phase testing
    • G01N33/54373—Apparatus specially adapted for solid-phase testing involving physiochemical end-point determination, e.g. wave-guides, FETS, gratings

Definitions

  • the invention is referred to a device enabling the increase of the sensitivity of sensors, based on the surface plasmon excitation method, whereas such sensors may be used in relation to the molecular adsorption on either free or suitably modified surfaces.
  • surface plasmon excitation Apart from the detection of surface plasmon excitation through the change of the incident angle of the light beam, this is also possible by other methods, as for example, by the change of the wavelength of the light beam.
  • the properties of surface plasmons (for example, the excitation frequency) are strongly related to the dielectric properties (refractive index) of the material surrounding the metallic film at a distance up to 200nm from the metallic surface. This strong dependence of surface plasmon properties has been widely used for the study of interfaces as well as for the study of adsorbed molecules phenomena on surfaces and for biological applications such as the detection of chemical relationship among biomolecules (Homola J.; Yee S. S.; Gauglitz G., Sensors and Actuators B: Chemical 54, 3-15 (1999)).
  • the adsorption of molecules on the free or modified metallic surface is accompanied by a very small change of the refractive index near the metallic surface, due to small amount of mass adsorbed on the said surface, which results in hardly detectable changes of the excitation curve before and after the adsorption.
  • detection of molecules that cannot be adsorb on the surface is desired.
  • the initially free (unmodified surface) is modified by an adsorbed layer of molecules on which modified surface the said molecules can be attached by some chemical reaction. It is clear that in such cases it would be necessary to invent a way for the enhancement of those changes.
  • the enhancement of changes appearing on the excitation curve can be achieved by an artificial increase of the surface available for molecular adsorption in the vicinity of (near) the metallic surface.
  • this is achieved by the creation of a layer of porous medium adjacent to (i.e. on top of) the metallic surface (i.e metallic film) on which takes place the excitation of surface plasmons.
  • This porous medium the total surface of which is much larger than that of the metallic surface is used subsequently for the detection of molecules to be adsorbed at a next step.
  • the active surface is much larger than the surface of the non-porous metal surface. In this way the adsorbed quantities are larger and consequently the displacements of the surface plasmon excitation curves are much larger compared to the case of adsorption on a non-porous surface.
  • the size of the pores which is controlled by its fabrication conditions, determines the size of the molecules which are able to penetrate into the pores. In this way the selective adsorption of molecules according to their size is enabled. Due to this property the new device can also be used as a selective sensor for toxic, biological or other molecules when there is a difference between the size of these molecules and the molecules of the environment in which they are dissolved. This condition is fulfilled in many situations where the molecules' environment is for example air, water or organic solvents.
  • Figure 1 shows a glass prism (1), which has adjacent to one of his sides a metal film (3). Adjacent to said metal film (3) is a porous medium (2). A light beam (4) enters the prism and after total reflection exits on a detector (5).
  • the present invention discloses a device for the enhancement of sensitivity of sensors by excitation of surface plasmons, which device comprises a glass prism or glass slide, a metal film, and a porous medium, wherein a side of the said glass prism or glass slide is adjacent to the one side of the metal film, and the other side of the said metal film is adjacent to said porous medium which porous medium covers the whole said surface of the metal film.
  • metal film of the device disclosed in the present invention is made of aluminium.
  • the porous medium is alumina.
  • the present invention also discloses a method of fabrication of the device of the invention, comprising anodisation for the formation of porous medium, wherein the anodisation process is interrupted at appropriate timing, before the complete anodiosation of the metal film.
  • the nature of the porous medium and the sizes of the pores determine the size of the molecules to be absorbed.
  • adsorption of the molecules takes place when the said molecules are in liquid or gaseous solutions.
  • toxic, biological or other molecules are selectively sensed.
  • a thin aluminium film is deposited by thermal evaporation under vacuum, whereas the thickness of the aluminium film is in the range between 60nm to 85 nm.
  • the said thin aluminium film can be deposited on a flat glass slide. Then the prism or the glass slide is immersed in an electrochemical cell of sulphuric acid aqueous solution 6% (at weight) and at a temperature of 10 0 C. The aluminium film is connected to a cable and it constitutes the anode of the element.
  • the cathode is constituted by a platinum leaf or mesh.
  • a constant potential difference of 20 V is applied between the anode and the cathode.
  • the curve of current is recorded and at appropriate timing the process is interrupted, before the complete anodiosation of the aluminium film.
  • the surface is rinsed with deionised water and then with ethanol, followed by the drying of the surface by blowing with nitrogen gas.
  • a layer of porous alumina (2) is created, while also a thin layer of aluminium remains in contact with (adjacent to) the surface of prism (or the glass slide) (3) due to the interruption of the said anodiosation process.
  • the surface plasmons are to be excited on this layer of aluminium, while in the porous alumina is realised the adsorption of molecules that we wish to detect and of which we wish to measure the adsorption.
  • the pores created may have depth 100-150nm, diameter from 14 up to 16 nm and they are arranged to be distanced from each other an average distance of 40 nm.
  • the said size of pores is suitable for the adsorption of molecules of the oligomer decaoctanic phosphoric acid (size of molecule 2 nm roughly).
  • the following process may be followed, which concerns the description of measurement of adsorption of decaoctanic phosphoric acid in porous and non-porous alumina surfaces.
  • the porous surface that has been created on the prism (or glass slide) in the previous stage is immersed in a bath of solution 0.1% at weight of decaoctanic phosphoric acid in ethanol.
  • the submersion is realised in room temperature and lasts 24 hours.
  • the prism (or glass slide) is removed from the bath; the surface is rinsed with ethanol and dried in nitrogen gas.
  • the prism (or the flat slide which comes into contact with the prism via a refractive index matching fluid) is placed in suitable apparatus for the excitation and detection surface plasmons. More specifically, a monochromatic beam of light, p - polarised (4) is directed to one of the two free faces of the prism. The said beam enters the prism, it is directed to the metallised face, where it suffers total reflection and comes out from the third face.
  • the out-coming beam falls on a suitable detector (5) which transforms the optical signal to an electrical one, and which is recorded continuously.
  • the prism and the detector are placed on a suitable goniometer [theta]/2 [theta] ⁇ /2 ⁇ , so while the angle of incidence of the incoming beam changes continuously, the out-coming beam is always directed to the detector.

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  • Health & Medical Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

A device consisting of a porous medium (2) in contact with a thin metallic film (3) on which surface plasmons are excited. The aim of the device is to enhance the changes of the surface plasmon excitation curve due to the adsorption of molecules on the porous surface in comparison with corresponding adsorption on the non-porous surface. Adsorption occurs on the free or on suitably modified surface of the porous media, either from liquid or gaseous phase. Detection is realized by recording and processing of the surface plasmon excitation curve under internal total refection conditions. The use of porous medium in contact with the metallic film, results in an enhancement in the change of the excitation curve by at least a factor of 10 in comparison with the adsorption on a non-porous surface.

Description

PROBES OF ENHANCED SENSITIVITY FOR ADSORBED MOLECULES
DETECTION
The invention is referred to a device enabling the increase of the sensitivity of sensors, based on the surface plasmon excitation method, whereas such sensors may be used in relation to the molecular adsorption on either free or suitably modified surfaces.
PRIORART Surface plasmon spectroscopy is an optical technique based on the collective excitation of the free electrons on the surface of a thin metallic film, which collective excitation is called "surface plasmons"
A number of different methods for the excitation of surface plasmons are described in the literature. According to one of those, namely the Kretchmann geometry, (H. Kretschmann, H. Raether. Z. Naturforsch 23a, 2135 (1968)), surface plasmons are excited on the surface of a thin metallic film which lies on the face of a glass prism. A monochromatic light beam under total internal reflection conditions is used for the plasmon excitation. The detection of the excitation is realised by the intense drop in the measured intensity of the monochromatic light beam which is reflected from the metallic film, versus the angle of incidence (excitation curve)
Apart from the detection of surface plasmon excitation through the change of the incident angle of the light beam, this is also possible by other methods, as for example, by the change of the wavelength of the light beam. The properties of surface plasmons (for example, the excitation frequency) are strongly related to the dielectric properties (refractive index) of the material surrounding the metallic film at a distance up to 200nm from the metallic surface. This strong dependence of surface plasmon properties has been widely used for the study of interfaces as well as for the study of adsorbed molecules phenomena on surfaces and for biological applications such as the detection of chemical relationship among biomolecules (Homola J.; Yee S. S.; Gauglitz G., Sensors and Actuators B: Chemical 54, 3-15 (1999)).
In several cases the adsorption of molecules on the free or modified metallic surface (either from liquid or from gaseous environment) is accompanied by a very small change of the refractive index near the metallic surface, due to small amount of mass adsorbed on the said surface, which results in hardly detectable changes of the excitation curve before and after the adsorption. This is also the case where detection of molecules that cannot be adsorb on the surface, is desired. Then the initially free (unmodified surface), is modified by an adsorbed layer of molecules on which modified surface the said molecules can be attached by some chemical reaction. It is clear that in such cases it would be necessary to invent a way for the enhancement of those changes.
The enhancement of changes appearing on the excitation curve can be achieved by an artificial increase of the surface available for molecular adsorption in the vicinity of (near) the metallic surface. According to the present invention, this is achieved by the creation of a layer of porous medium adjacent to (i.e. on top of) the metallic surface (i.e metallic film) on which takes place the excitation of surface plasmons. This porous medium, the total surface of which is much larger than that of the metallic surface is used subsequently for the detection of molecules to be adsorbed at a next step. As the inner walls of the pores are also available for accommodating adsorbed molecules, the active surface is much larger than the surface of the non-porous metal surface. In this way the adsorbed quantities are larger and consequently the displacements of the surface plasmon excitation curves are much larger compared to the case of adsorption on a non-porous surface.
Additionally, the size of the pores, which is controlled by its fabrication conditions, determines the size of the molecules which are able to penetrate into the pores. In this way the selective adsorption of molecules according to their size is enabled. Due to this property the new device can also be used as a selective sensor for toxic, biological or other molecules when there is a difference between the size of these molecules and the molecules of the environment in which they are dissolved. This condition is fulfilled in many situations where the molecules' environment is for example air, water or organic solvents.
Description of the device of the invention with an example of its manufacturing and use, with reference to the attached drawing.
The invention is illustrated through Figure 1 which shows: Figure 1 shows a glass prism (1), which has adjacent to one of his sides a metal film (3). Adjacent to said metal film (3) is a porous medium (2). A light beam (4) enters the prism and after total reflection exits on a detector (5).
With No (6) is illustrated a section of the pores of the porous medium before the adsoption of the molecules, while with No. (7) is illustrated the same section after the adsoption of the molecules.
The present invention discloses a device for the enhancement of sensitivity of sensors by excitation of surface plasmons, which device comprises a glass prism or glass slide, a metal film, and a porous medium, wherein a side of the said glass prism or glass slide is adjacent to the one side of the metal film, and the other side of the said metal film is adjacent to said porous medium which porous medium covers the whole said surface of the metal film.
Preferably, metal film of the device disclosed in the present invention is made of aluminium.
Advantageously, the porous medium is alumina.
The present invention also discloses a method of fabrication of the device of the invention, comprising anodisation for the formation of porous medium, wherein the anodisation process is interrupted at appropriate timing, before the complete anodiosation of the metal film.
Advantageously, for the detection of adsorbed molecules by surface plasmon excitation with use of the device of the present invention, the nature of the porous medium and the sizes of the pores determine the size of the molecules to be absorbed.
Conveniently, for the detection of adsorbed molecules by surface plasmon excitation with use of the device of the present invention, adsorption of the molecules takes place when the said molecules are in liquid or gaseous solutions.
Preferably, for the detection of adsorbed molecules by surface plasmon excitation with use of the device of the present invention, toxic, biological or other molecules are selectively sensed.
Advantageously, for the use of the device of the present invention this may be adapted in any detecting system. Where in the present description we mention prism, we mean a glass prism. EXAMPLE:
The fabrication of the proposed device can be completed in the following procedure: Preferably, on one face of a prism (1) a thin aluminium film is deposited by thermal evaporation under vacuum, whereas the thickness of the aluminium film is in the range between 60nm to 85 nm.
Alternatively, the said thin aluminium film can be deposited on a flat glass slide. Then the prism or the glass slide is immersed in an electrochemical cell of sulphuric acid aqueous solution 6% (at weight) and at a temperature of 10 0C. The aluminium film is connected to a cable and it constitutes the anode of the element.
The cathode is constituted by a platinum leaf or mesh. A constant potential difference of 20 V is applied between the anode and the cathode. The curve of current is recorded and at appropriate timing the process is interrupted, before the complete anodiosation of the aluminium film. After the anodiosation the surface is rinsed with deionised water and then with ethanol, followed by the drying of the surface by blowing with nitrogen gas. With the anodiosation process a layer of porous alumina (2) is created, while also a thin layer of aluminium remains in contact with (adjacent to) the surface of prism (or the glass slide) (3) due to the interruption of the said anodiosation process.. The surface plasmons are to be excited on this layer of aluminium, while in the porous alumina is realised the adsorption of molecules that we wish to detect and of which we wish to measure the adsorption. The pores created may have depth 100-150nm, diameter from 14 up to 16 nm and they are arranged to be distanced from each other an average distance of 40 nm. The said size of pores is suitable for the adsorption of molecules of the oligomer decaoctanic phosphoric acid (size of molecule 2 nm roughly).
With regard to the use of the device for the detection of adsorption phenomena, the following process may be followed, which concerns the description of measurement of adsorption of decaoctanic phosphoric acid in porous and non-porous alumina surfaces. The porous surface that has been created on the prism (or glass slide) in the previous stage is immersed in a bath of solution 0.1% at weight of decaoctanic phosphoric acid in ethanol. The submersion is realised in room temperature and lasts 24 hours. Afterwards the prism (or glass slide) is removed from the bath; the surface is rinsed with ethanol and dried in nitrogen gas. During the submersion, molecules of decaoctanic phosphoric acid penetrate in the interior of the porous media and are adsorbed on the available surfaces. In Figure 1 is shown a section of porous alumina before adsorption (6) and the same region after the adsorption of molecules of decaoctanic phosphoric acid (7).
The same process may be also followed in the case of use of a flat non- porous surface of alumina for the adsorption of decaoctanic phosphoric acid in order to stress the advantage of the proposed device.
For the measurement procedures, the prism (or the flat slide which comes into contact with the prism via a refractive index matching fluid) is placed in suitable apparatus for the excitation and detection surface plasmons. More specifically, a monochromatic beam of light, p - polarised (4) is directed to one of the two free faces of the prism. The said beam enters the prism, it is directed to the metallised face, where it suffers total reflection and comes out from the third face. The out-coming beam falls on a suitable detector (5) which transforms the optical signal to an electrical one, and which is recorded continuously. The prism and the detector are placed on a suitable goniometer [theta]/2 [theta] Θ/2Θ, so while the angle of incidence of the incoming beam changes continuously, the out-coming beam is always directed to the detector.
In this way the curve of excitation of surface plasmons is recorded and it is compared to the corresponding curve for the free surface (without adsorbed molecules). A shift of the curve of excitation is observed in the order of two degrees. This shift in the case of adsorption in porous alumina is roughly ten times bigger compared to the one that is measured when non- porous solid surface of alumina is used.
It is obvious that with the sensor proposed with the present invention, there is a big enhancement of the shift of the excitation curve, which is related with the phenomenon of adsorption, and consequently increases the sensitivity of the above-mentioned surface plasmon excitation device.

Claims

1. Device for the enhancement of sensitivity of sensors by excitation surface plasmons, comprising a glass prism or glass slide
- a metal film, a porous medium, characterised in that a side of the said glass prism or glass slide is adjacent to the one side of the metal film,
- the other side of the said metal film is adjacent to said porous medium which porous medium covers the whole said surface of the metal film.
2. Device according to Claim 1, characterised in that the metal film is made of aluminium.
3. Device according to Claim 1, characterised in that the porous medium is alumina.
4. Method of fabrication of the device according to any one of Claims 1 to 3, comprising anodisation for the formation of porous medium, characterized in that the anodisation process is interrupted at appropriate timing, before the complete anodiosation of the metal film.
5. Detection of adsorbed molecules by surface plasmon excitation with use of the device in Claims 1 to 3, characterised in that the nature of the porous medium and the sizes of the pores determine the size of the molecules to be absorbed.
6. Detection of adsorbed molecules by surface plasmon excitation according to Claim 5, characterised in that adsorption of the molecules takes place when the said molecules are in liquid or gaseous solutions.
7. Detection of adsorbed molecules by surface plasmon excitation according to Claims 5 or 6, characterised in that toxic, biological or other molecules are selectively sensed.
8. Use of the device of any of claims 1 to 8, characterised in that such device is adapted in any detecting system.
PCT/GR2008/000052 2007-08-02 2008-07-22 Probes of enhanced sensitivity for adsorbed molecules detection WO2009016419A1 (en)

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GR20070100496A GR20070100496A (en) 2007-08-02 2007-08-02 Arrangement increasing the sensitivity of sensors based on the surface plasmons stimulation phenomenon used for the detection of absorbed molecules
GR20070100496 2007-08-02

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2372343A1 (en) * 2010-02-25 2011-10-05 Stichting IMEC Nederland Gas sensor, method for optically measuring the presence of a gas using the gas sensor and gas sensing system
US8711356B2 (en) 2010-02-25 2014-04-29 Stichting Imec Nederland Gas sensor with a porous layer that detectably affects a surface lattice resonant condition of a nanoparticle array

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2372343A1 (en) * 2010-02-25 2011-10-05 Stichting IMEC Nederland Gas sensor, method for optically measuring the presence of a gas using the gas sensor and gas sensing system
US8711356B2 (en) 2010-02-25 2014-04-29 Stichting Imec Nederland Gas sensor with a porous layer that detectably affects a surface lattice resonant condition of a nanoparticle array

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