Method for producing a chromatography analysis column

Patent metadata

Field	Value
Publication number	US-9835599-B2
Application number	US-201314414848-A
Country	US
Kind code	B2
Filing date	Jul 2, 2013
Priority date	Jul 19, 2012
Publication date	Dec 5, 2017
Grant date	Dec 5, 2017

Abstract

The invention concerns a method for producing a chromatography analysis column, the resulting column, and a device comprising such a column. The method according to the invention comprises the following steps: (a) depositing on the flat surface of a substrate a first layer of particles which are intended to form the stationary phase; (b) depositing on the layer at least one second layer of compactly assembled particles; (c) impregnating the first and second layers with a light radiation-sensitive material, to form at least two compactly assembled particle layers impregnated with sensitive material; (d) insolating these layers in the regions corresponding to the desired internal shape of the chromatography analysis column, if the light radiation-sensitive material behaves like a positive resin, or outlining this internal shape if the light radiation-sensitive material behaves like a negative photosensitive resin; (e) eliminating either the regions insolated in step (d) if the light radiation-sensitive layer behaves like a positive photosensitive resin, or the regions not insolated in step (d) if the light radiation-sensitive material behaves like a negative photosensitive resin; and (f) covering and sealing the structure obtained in step (e) with a cover covered on the face facing the layers with at least one layer of compactly assembled particles which are identical to or different from those deposited on the substrate surface. The invention is used in particular in the field of chemical analysis.

First claim

The invention claimed is:

1. A process for the manufacture of a chromatography analytical column of the open tube having a porous layer type, characterized in that it comprises the following steps:
a) deposition of a first layer ( 2 ) of identical or different particles, which are intended to form the stationary layer, on the flat surface of a substrate ( 1 ),
b) deposition of at least one second layer ( 12 ) of particles as a compact assemblage on the layer ( 2 ),
c) impregnation of the layers ( 2 , 12 ) with a material sensitive to light radiation ( 4 ), in order to form at least two layers ( 3 ) of particles as a compact assemblage impregnated with sensitive materials,
d) insolation of the layers ( 3 ) in the regions corresponding to the internal shape desired for the chromatography analytical column, when the material sensitive to light radiation ( 4 ) behaves as a positive resin, or outlining this internal shape, when the material sensitive to light radiation ( 4 ) behaves as a negative photosensitive resin,
e) removal:
of the regions insolated in step d), when the material sensitive to light radiation ( 4 ) behaves as a positive photosensitive resin, or
of the regions not insolated in step d), when the material sensitive to light radiation ( 4 ) behaves as a negative photosensitive resin, and

f) covering and sealing the structure obtained in step e) with a covering cap ( 7 ) covered, on its face turned towards the layers ( 3 ), with at least one layer of particles as a compact assemblage identical to or different from those deposited on the surface of the substrate ( 1 ).

2. The process as claimed in claim 1 , characterized in that it additionally comprises, before step a), a step a1) of activation of said surface of the substrate ( 1 ), preferably by O2 plasma, UV radiation, a mixture of sulfuric acid and of hydrogen peroxide, or ozone.

3. The process as claimed in claim 2 , characterized in that it additionally comprises, after step a1) of activation of said surface of the substrate ( 1 ), a step a2) of thermal annealing of said surface of the substrate ( 1 ) which has been subjected to step a1).

4. The process as claimed in claim 1 , characterized in that it additionally comprises, after step c) of impregnation of the layers ( 2 ), a step c1) of thermal annealing of the substrate ( 1 ) and of the layers ( 3 ).

5. The process as claimed in claim 1 , characterized in that it additionally comprises, after step d) of insolation of the layers ( 3 ), a step d1) of thermal annealing of the substrate ( 1 ) coated with the insolated layers ( 3 ).

6. The process as claimed in claim 1 , characterized in that it additionally comprises, after step e) of removal of the insolated or non-insolated regions, a step e1) of annealing of the substrate ( 1 ) covered with the layers ( 3 ), certain regions of which have been removed.

7. The process as claimed in claim 1 , characterized in that it additionally comprises a step of formation of at least one layer of particles as a compact assemblage on a face of the covering cap ( 7 ).

8. The process as claimed in claim 1 , characterized in that said particles have a mean diameter of between 50 nm and 500 μm inclusive.

9. The process as claimed in claim 1 , characterized in that the total thickness of the layers ( 2 , 12 ) is between 50 and 700 μm inclusive.

10. The process as claimed in claim 1 , characterized in that the particles are particles made of a metal oxide, or made of a ceramic, or made of a polymer, or made of a polysaccharide, or made of a metal; these particles optionally being functionalized.

11. The process as claimed in claim 1 , characterized in that step a) is carried out by the Langmuir-Blodgett method, or by the Langmuir-Schaefer method, or by Marangoni self-assembling, or by the vortical surface method, or by floating-transferring, or by dip coating, or by spin coating.

12. The process as claimed in claim 1 , characterized in that the material sensitive to light radiation ( 4 ) behaves as a positive resin and is sensitive to radiation with wavelengths of between 150 and 700 nm inclusive.

13. The process as claimed in claim 1 , characterized in that the material sensitive to light radiation ( 4 ) behaves as a negative resin and is sensitive to radiation with wavelengths of between 150 and 700 nm inclusive.

14. The process as claimed in claim 1 , characterized in that the material sensitive to light radiation ( 4 ) is obtained by a sol-gel process.

15. The process as claimed in claim 1 , characterized in that step c) is carried out by spin deposition of the material sensitive to light radiation ( 4 ) on the layer ( 2 ) or by immersion of the substrate ( 1 ) coated with the layer ( 2 ) in the material sensitive to light radiation ( 4 ).

16. The process as claimed in claim 1 , characterized in that step d) of insolation of the layers ( 3 ) with the light radiation ( 4 ) is carried out through a mask ( 11 ) comprising regions transparent to said light radiation ( 4 ), these transparent regions corresponding to:
the internal shape desired for the chromatography analytical column, when the material sensitive to light radiation ( 4 ) behaves as a positive resin, or
outlining this internal shape, when the material sensitive to light radiation ( 4 ) behaves as a negative resin.

17. The process as claimed in claim 1 , characterized in that step d) of insolation of the layers ( 3 ) is carried out by laser writing in order to form the internal shape desired for the column, when the material sensitive to light radiation ( 4 ) behaves as a positive resin, or in the regions outlining this internal shape, when the material sensitive to light radiation ( 4 ) behaves as a negative resin.

18. The process as claimed in claim 1 , characterized in that the substrate is rigid or flexible and made of a material chosen from a metal oxide, a metal, a ceramic or a polymer.

19. The process as claimed in claim 1 , characterized in that the particles are made of a material chosen from silica, titanium dioxide, alumina, latex, polydimethylsiloxane (PDMS), gold, copper and the mixtures of these.

20. A chromatography analytical column, characterized in that it comprises a substrate ( 1 ), a flat surface of which is coated with at least one layer ( 3 ) of particles, this layer ( 3 ) of particles, which are optionally functionalized, comprising a region ( 5 ) devoid of the particles and forming the internal portion of the column and in that at least one wall of the column consists of a mixture of said particles, which are optionally functionalized, and of a material sensitive to light radiation, which is crosslinked.

21. The column as claimed in claim 20 , characterized in that the particles are particles made of a metal oxide, polymer, polysaccharide, metal or ceramic, these particles optionally being functionalized.

22. The column as claimed in claim 20 , characterized in that the particles have a mean diameter of between 50 nm and 500 μm inclusive.

23. The column as claimed in claim 20 , characterized in that the substrate ( 1 ) is flexible or rigid and is made of a material chosen from a metal oxide, a metal, a ceramic or a polymer.

24. The column as claimed in claim 20 , characterized in that the particles are made of a material chosen from silica, alumina, titanium oxide, latex, polydimethylsiloxane (PDMS), gold, copper or mixtures of these.

Assignees

• Commissariat Energie Atomique

Inventors

• Dellea Olivier
• Fugier Pascal
• Marie Helene
• Vignoud Severine

Classifications

• B01D53/025

  with wetted adsorbents; Chromatography (analytical chromatography G01N30/00 - G01N30/96; for liquids B01D15/08) · CPC title

• B01J20/3204

  Inorganic carriers, supports or substrates · CPC title

• B01J20/3259

  comprising at least two different types of heteroatoms selected from nitrogen, oxygen or sulfur with at least one silicon atom · CPC title

• B01J20/282 Primary

  Porous sorbents (ion exchange B01J39/00 - B01J41/00) · CPC title

• B01J20/3219

  involving a particular spacer or linking group, e.g. for attaching an active group · CPC title