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(12) United States Patent (10) Patent No.: US 8,088,615 B2 Ausserre (45) Date of Patent: Jan

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(12) United States Patent (10) Patent No.: US 8,088,615 B2 Ausserre (45) Date of Patent: Jan USOO8088615B2 (12) United States Patent (10) Patent No.: US 8,088,615 B2 Ausserre (45) Date of Patent: Jan. 3, 2012 (54) OPTICAL COMPONENT FOR OBSERVINGA (56) References Cited NANOMETRIC SAMPLE, SYSTEM COMPRISING SAME, ANALYSIS METHOD U.S. PATENT DOCUMENTS USING SAME, AND USES THEREOF 5,639,671 A * 6/1997 Bogartet al. ................. 436,518 (76) Inventor: Dominique Ausserre, Soulitre (FR) 5,962,114 A * 10/1999 Jonza et al. ........ ... 428.212 6,034,775 A * 3/2000 McFarland et al. ............. 506/12 (*) Notice: Subject to any disclaimer, the term of this 6,312,691 B1 * 1 1/2001 Browning et al. ......... 424,143.1 patent is extended or adjusted under 35 6,493.423 B1* 12/2002 Bisschops .............. ... 378,119 U.S.C. 154(b) by 777 days. 6,697,194 B2 * 2/2004 Kuschnereitet al. ... 359,359 6,710,875 B1* 3/2004 Zavislan ............ ... 356,364 (21) Appl. No.: 11/631,846 6,718,053 B1 * 4/2004 Ellis et al. ... ... 38.2/128 Jul. 6, 2005 6,853,455 B1* 2/2005 Dixon et al. ... 356/453 (22) PCT Filed: 6,934,068 B2 * 8/2005 Kochergin ... ... 359,280 (Under 37 CFR 1.47) 7.209,232 B2 * 4/2007 Ausserre et al. 356,369 7,258,838 B2* 8/2007 Lietal. .......... ... 422.68.1 (86). PCT No.: PCT/FR2OOS/OO1746 7,265,845 B2 * 9/2007 Kochergin . ... 356,445 S371 (c)(1), * cited by examiner (2), (4) Date: Aug. 12, 2008 Primary Examiner — Sang Nguyen (87) PCT Pub. No.: WO2006/013287 (74) Attorney, Agent, or Firm — Blank Rome LLP PCT Pub. Date: Feb. 9, 2006 (65) Prior Publication Data (57) ABSTRACT US 2010/0062422 A1 Mar. 11, 2010 The invention concerns an optical component for observing a (30) Foreign Application Priority Data sample, which includes a Substrate and at least one complex indeX layer of predetermined thickness, designed to show a Jul. 7, 2004 (FR) ...................................... O4 O7517 high intensity or color contrast for optical path variations, (51) Int. Cl. reliefs, nanometric thicknesses and diameters when it is CI2O I/68 (2006.01) observed by incoherent light reflection convergent around the CI2M I/34 (2006.01) normal incidence under polarization extinction conditions. GOIJ 4/00 (2006.01) The upper indeX layer has specific Surface properties provid (52) U.S. Cl. .......................... 435/287.2:435/6: 356/369 ing it with selective affinity relative to at least one character (58) Field of Classification Search .................. 356/244, istic of the sample. An analysis system includes such a com 356/246, 445, 364-369; 435/287.1, 287.2, ponent, an analysis method using the component and uses of 435/287.7, 287.9; 436/518, 146, 172,524; the method. 422/82.05, 82.08, 82.11: 359/280, 359; 382/128, 382/255 See application file for complete search history. 61 Claims, 20 Drawing Sheets PART SHARED BY AND 20 -j-.5 60 -------- GEERA. ONE OF HE SYSE. FORANASSEY REFLECN OP:CALCOMPONENT 3. U.S. Patent Jan. 3, 2012 Sheet 1 of 20 US 8,088,615 B2 8 r & s a PART SHARED BY 10 AND 20 5 FIG. 1 80 - GENERA. ONE OF THE SYSTEM FOR ANAYSS BY REFECON OPTCACOMPONENT 30 OUTINE OF AN OPTICA COMPONEN ACCORONG ONENTO U.S. Patent Jan. 3, 2012 Sheet 2 of 20 US 8,088,615 B2 ESEEGNHSSYS ORENATON 100 OFCO OFCO SaaS ZOA TOFCO OFCO 4 SICON OFCO 5 SLICON OFCO OFCO Sara FIG. 2B WAROUS PROTOTYPES OF OPTICAL COMPONENS ACCORDING TO THE NVENTON U.S. Patent Jan. 3, 2012 Sheet 3 of 20 US 8,088,615 B2 FIG. 3 ASESSINGANASRAN BANE SGE OPCA COMPONENT ACCORDENGOENVENON FIG. 5 AGE OF A SPPORBAYER OBSERVE NERSON U.S. Patent Jan. 3, 2012 Sheet 4 of 20 US 8,088,615 B2 &D A. R 8.st CO& 0.BBXC FIG.4 OVERVIEW OF A MEMBRANE PROTEN SENSORFOR PRODUCNGA BOCHF WH PROENS U.S. Patent Jan. 3, 2012 Sheet 5 of 20 US 8,088,615 B2 5AMNO's ANZED optical componeNists 5S ARESPOTED AND JVCROSS-LINKED (SP) 1 Sp CONTROL SPSFREHYBROZED 2SF's ARE CHEMCALLY SF SprEHYBRZED WITH BSA (SPB) BLOCKED (SPC) WITHOUBSA (SPnB SPCsPREHYBRIZED 1 SPCCONTROL WITH BSA (SPCB) OBSERVATIONUSING OURTECHNOUEF Hybribization witHTHEE TARGETI HYBRDZATIONL E WITH THE TARGET WITH PRESENCE OF DEINHART WHOUTEENiART E. F. OBSERVATIONUSING OURTECHNOUE AND FOURESCENCE S W S S SS U.S. Patent Jan. 3, 2012 Sheet 6 of 20 US 8,088,615 B2 S. S S S. DETECTED NOT DETECTED FIG. 6G SUM OF THE Cy3 AND Cy5 FOURESCENCESIGNALS U.S. Patent Jan. 3, 2012 Sheet 7 of 20 US 8,088,615 B2 DETECTIONUSING OUR EO 8 AMOUNT OF 3 FLORESCENCE SIGNA, FIG. 6H DETECTED REPRESENAEON OF EVE OF TOTA NOT DETECTED FLORESCENCE NEACH OF THE SOS & S &SS yŠS $y S U.S. Patent Jan. 3, 2012 Sheet 8 of 20 US 8,088,615 B2 FIG. 7A 2D PROTSN CRYSTAS FIG. 7B 3 TN PROTEN CRYSAS -o-M-MFIG.7C 2D POLYMER CRYSTAS (POYETHYLENE GLYCOL 4000) U.S. Patent Jan. 3, 2012 Sheet 9 of 20 US 8,088,615 B2 F.G. 7D HREE-DENSONAVSUALIZATION OF HE CRYSA AION OF E SAME POLYMER (POLYEHYLENE GLYCOL 4000) ATROOM EMPERATURE U.S. Patent Jan. 3, 2012 Sheet 10 of 20 US 8,088,615 B2 FIG. 8 NSPECT ON, CONTROLAND FOOW-UP OFHE CRYSAZATION OF APROENGE OBSERVE U.S. Patent Jan. 3, 2012 Sheet 11 of 20 US 8,088,615 B2 ANALYss systEM F G 9 SUDYNG AND NSPECNG ANOUBES F G. 9B DETECTION OF CARBON NANOT BES WHRARE SHAPES U.S. Patent Jan. 3, 2012 Sheet 12 of 20 US 8,088,615 B2 FIG. 11A OFFERSNAL CONTRAS DEVICE U.S. Patent US 8,088,615 B2 U.S. Patent Jan. 3, 2012 Sheet 14 of 20 US 8,088,615 B2 FIG. 12 SYSE FOR if ASUREMENNOT AGERY 8ETWEEN CROSSED POLARZERS U.S. Patent Jan. 3, 2012 Sheet 15 of 20 US 8,088,615 B2 () SS S. % :? U.S. Patent Jan. 3, 2012 Sheet 16 of 20 US 8,088,615 B2 & Š s SS Š s S y S U.S. Patent Jan. 3, 2012 Sheet 17 of 20 US 8,088,615 B2 FG. 15A U.S. Patent Jan. 3, 2012 Sheet 18 of 20 US 8,088,615 B2 15B Li C2 17 U.S. Patent Jan. 3, 2012 Sheet 19 of 20 US 8,088,615 B2 FIG 18A FIG. 19 U.S. Patent Jan. 3, 2012 Sheet 20 of 20 US 8,088,615 B2 FIG.2OB US 8,088,615 B2 1. 2 OPTICAL COMPONENT FOR OBSERVING A The component according to the invention makes it pos NANOMETRIC SAMPLE, SYSTEM sible to deduce from optical observation the characteristics COMPRISING SAME, ANALYSIS METHOD corresponding to the affinity with all or part of the surface of USING SAME, AND USES THEREOF the optical component containing the sample. 5 Advantageously: The present invention relates to the field of observation and said sample is observed under differential interference con analysis of nanometric characteristics using an optical com trast, ponent and a polarised light observation system. said Surface properties have affinity characteristics that Known in the state of the art is the technology that consists vary according to the coordinates on the Surface of the of preparing a sample Support plate having indeX layers that 10 component, meet specific conditions, such as provided in patents the optical characteristics of the component vary according FR2818376 and FR284.1339. to the coordinates of the area being considered on the Also known in the state of the art is U.S. Pat. No. 5,631, Surface of the component, 171, describing equipment for observing nanometric thick the variations of the optical characteristics of the compo ness differences, by analysing the refraction of thin layers. 15 nent and the variations of the Surface properties are These various solutions require the design and production correlated, of a specific plate for each type of sample to be observed, and said variations form a gradient following at least one direc do not make it possible to conduct studies of undetermined tion of the optical component, samples or those with variable characteristics. said variations are Sudden, thereby delimiting clearly sepa The present invention aims to solve these disadvantages by rate domains on the Surface Such as, for example, in the providing a solution that makes it possible to develop a broad case of biochips, artificial noses, hydrophilic/hydropho range of applications for studying samples in which certain bic boundaries or, in general terms, Surface patterns. characteristics are not known, by observing their optical and said variations constitute even paving of the Surface, physical characteristics. said variations constitute a matrix network, The invention relates, according to its most general sense, 25 the component has visible markers that make it possible to to an optical component for observing a sample, comprising identify and locate a specific area. a Substrate and at least one complex indeX layer of predeter According to the invention, the Surface of the optical com mined thickness, designed to show a high intensity or colour ponent has affinity properties that correspond to non-constant contrast for optical path variations, reliefs, nanometric thick physical, chemical or biological characteristics. These affin nesses and diameters when it is observed by incoherent light 30 ity properties can consist of Surface energy, Surface electrical reflection convergent around the normal incidence under charge, Surface polarisability, selective porosity, physical polarisation extinction conditions, characterised in that the affinity, physical-chemical affinity, capture and/or recogni upper indeX layer has specific Surface properties providing it tion sites, liquid film, presence of a solution, magnetic agents, with selective affinity relative to at least one characteristic of Surface active agents, textures, chemical reaction cells, selec the sample.
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