WO2001038857A1 - Optical sensors and arrays containing thin film electroluminescent devices - Google Patents
Optical sensors and arrays containing thin film electroluminescent devices Download PDFInfo
- Publication number
- WO2001038857A1 WO2001038857A1 PCT/US2000/031921 US0031921W WO0138857A1 WO 2001038857 A1 WO2001038857 A1 WO 2001038857A1 US 0031921 W US0031921 W US 0031921W WO 0138857 A1 WO0138857 A1 WO 0138857A1
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- WO
- WIPO (PCT)
- Prior art keywords
- optical sensor
- sensor according
- thin film
- biphenyl
- optical
- Prior art date
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Classifications
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
-
- 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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/66—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light electrically excited, e.g. electroluminescence
-
- 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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/7703—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator using reagent-clad optical fibres or optical waveguides
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2201/00—Features of devices classified in G01N21/00
- G01N2201/06—Illumination; Optics
- G01N2201/062—LED's
- G01N2201/0628—Organic LED [OLED]
Definitions
- TFELD fluorescence-activated optical sensors, probes, and integrated multiprobe
- Optical sensing and probing is an alternative to electrochemical sensors
- Such affects may include a change in the PL
- inorganic single crystal III-V compound LEDs as the light source.
- the sensor and to collect the PL for readout increases complexity, size,
- Single crystal GaN-based inorganic LEDs also are incompatible
- U.S. Patent No. 5,517,313 relates to an optical sensor using a
- P-N junction as a light emitting diode.
- the LED is placed in an indicator
- the emitted light is incident upon a photodetector.
- an optical sensing device which includes a light- emitting P-N junction
- the hole contains an analyte-
- a photodetector at one end of the hole generates an electrical signal responsive to light emitted by the fluorescent
- P-N junction LEDs are typically prepared from
- P-N junction LEDs cannot be made transparent to allow
- P-N junction LEDs are fabricated at temperatures
- TFELD fluorescent light emitting diode
- arrays capable of monitoring, quantifying, and analyzing analytes in real ⁇
- the present invention provides optical sensors, probes and
- the sensors, probes, and sensors are range of biological, chemical, and physical analytes.
- the sensors, probes, and sensors are a range of biological, chemical, and physical analytes.
- the sensors, probes, and sensors are a range of biological, chemical, and physical analytes.
- arrays include an analyte-sensitive layer optically coupled to a thin
- the TFELD may be deposited on one
- the surface of the substrate supports a sensor layer such that the sensor layer
- the sensor layer and TFELD are thus in face-to-face
- the TFELD is
- the optical response varies
- the response is detected by a
- the invention also provides arrays containing large numbers of
- sensor pixels and corresponding TFELDs prepared on-chip in microelectronic configurations.
- sensor units prepared on-chip in microelectronic configurations.
- TFELDs such as organic light emitting devices
- OLED optical detector
- back detection herein we mean that the photodetector is located on
- the devices of the invention are
- the sensor layer may be, e.g., a thin
- the Ru(dpp) sensor layer may be
- biosensors which utilize sensing strategies and indicator systems for
- TFELD-activated ion correlation sensors TFELD-activated ion correlation sensors, enzymatic sensors,
- Real-time readout obviates the need to send a measuring device
- curative action can be taken at once, rather than waiting for receipt of the
- the sensing chemistry can be selected to depend on the
- the disposable integrated probe or sensor is easily replaceable.
- the invention are constructed such that the TFELD light source and the
- each sensor unit is comprised of two
- thin film layers analyte-sensitive sensor layer and TFELD
- protective clothing can obtain real-time information on the condition of
- the invention provides miniature
- disposable sensors are provided to form a "first aid sensor kit" to be applied to and around the location of
- FIG. 1 shows a schematic of an integrated OLED probe
- FIG. 2 depicts an optical sensor according to the invention
- FIG. 3 shows a schematic of the EL and PL light pathways of
- FIG. 4 depicts an optical sensor according to the invention
- FIG. 5 shows a schematic of the EL and PL light pathways of
- FIG. 6 depicts a sensor according to the invention in back
- FIG. 7 shows a schematic of the EL and PL light pathways of
- FIG. 8 depicts a multisensor array according to the invention.
- FIG. 9 shows the electroluminscence of a blue OLED under a
- FIG. 10 shows the excitation, absorption, and PL spectra of an
- Ru(dpp) dye immobilized within a sol-gel matrix.
- the PL is shown in
- FIG. 11 shows the PL of an Ru(dpp) oxygen sensor excited by
- FIG. 12 shows the change in PL intensity of an Ru(dpp)
- oxygen sensor as a reaction to change in oxygen concentration, excited by
- FIG. 13 shows time-resolved PL and EL collected in direct
- FIG. 14 shows time-resolved and spectrally-resolved PL and EL
- FIG. 15 shows time-resolved and spectrally-resolved PL and EL
- FIG. 16 shows the time-resolved and spectrally-resolved PL
- present invention combine thin layer probing and sensing chemistries and light sources (TFELDs), which may be arranged face-to-face in contact
- the probe or sensor layer may be deposited directly on the
- the probe or sensor is exposed to the analyte, while the light
- the source is preferably sealed from the analyte by the substrate or a suitable
- Each probe or sensor unit contains a selective indicator
- the probe or sensor relies upon d e optical
- optical signal generation of the probe or sensor can be accomplished using
- indicator agents including colorimetric or
- fluorescent dyes selective polymer films, or biological receptors such as
- At least one probe or sensor is provided.
- each analyte or Ugand of interest is provided for the detection of each analyte or Ugand of interest.
- Some of the sensor units may also use indicator agents which serve as an
- Individual sensing elements may be paired with individual
- TFELDs preferably selected such that the absorption coefficient of the indicator agent and/or sensor layer is relatively high at the emission peak
- each probe or sensor unit typically includes
- a transparent substrate 1 which has a probe or sensor layer 2
- TFELD generally shown as 4, including luminescent layer 5,
- bias from wire 8 is applied to the cathode 7 and a positive bias, from wire 8.
- electroluminescent light 94 of a predetermined wavelength through
- the analyte may be detected by measuring the wavelength
- Each probe or sensor layer 2 comprises a thin film formed by,
- a polymeric matrix for example, a polymeric matrix, support, or other carrier, and an
- indicator agent such as a dye, and typically appears as a discrete film
- optical density i.e., absorbance
- the thin film probing or sensing layer 2 typically has a regular
- the flexibility and tensile strength of the thin film may vary
- the supporting substrate 1 may also take any size,
- configuration, or appearance may be geometrically regular or irregular
- substrate 1 is a translucent or transparent article such that light may pass
- an optically active material such as a
- the supporting substrate 1 serves as a physical location and/or a guide to the PL and EL emissions
- the probe or sensor units may be fabricated by first
- the probe or sensor layer and/or TFELD may be
- the TFELD 4 may likewise be prefabricated and
- luminescent active layer typically they are less than about 1 ⁇ in
- TFELDs may be low or high voltage, single crystal, poly crystalline, or
- amorphous may be prepared as extended area devices and operated by
- TFELDs can be inorganic
- an inorganic solid-state TFELD includes elements from Groups IIB, IIIA, rVA, and VA of the Periodic Table of the Elements.
- the elements from Groups IIB, IIIA, rVA, and VA of the Periodic Table of the Elements.
- the elements from Groups IIB, IIIA, rVA, and VA of the Periodic Table of the Elements.
- TFELD can be made of polycrystalline zinc sulfide (ZnS) or selenide
- TFELDs can be based on organic molecules as well. Because of
- injection EL high applied field
- P3ATs poly(3-alkylthiophenes)
- the TFELD of the sensor unit is at least 90% transmissive
- the TFELD is preferably
- TFELD 4 comprises an anode 6 on
- Anode 6 typically
- CuPc copper phthalocyanine
- hole transporting layer 10 In a particularly preferred embodiment, hole transporting layer
- hole transporting layer being made of N,N',biphenyl-N,N'-bis(3-
- Either or both hole transporting layers may also comprise
- Emitting Diode with Improved Color Purity Using a LiF/Al Cathode is a LiF/Al Cathode
- Electron transporting layer 5 is deposited on hole-
- transporting layer 10 one or preferably both of layers 5 and 10 being
- transporting layer 5 preferably comprises 8-tris-(hydroxy quinoline) Al
- Alq 3 (green emitter), amino oxadiazolefluorene (“AODF”) (blue
- CBP 4,4'-N,N'-dicarbazolyl biphenyl
- DSA distyrylarylene
- Electrophosphorescent Devices Appl. Phys. Lett. 74, 442 (1999).
- Cathode 7 preferably a thin film of lithium fluoride, or cesium fluoride,
- cathode 7 generating visible radiation 94.
- TFELD TFELD
- the devices according to the invention may be constructed
- TFELD may be modified, e.g., by fabricating the TFELD in a ring or horseshoe
- Cathode 15 causes electroluminescent layer 16 to
- an analyte-containing medium 18 such as
- the direct transmission embodiment is also shown in Figure 3.
- Figure 3 shows a device containing a substrate 20, and an
- Electrode 23 is
- electroluminescent and sensor layers 21 and 23 are in face-to-face
- the sensor layer 21 is exposed to analyte as shown
- PL 25 passes through filter 26 for filtering out any undesired
- the PL 25 is then collected by a photodetector 27, such as a Si
- photodiode avalanche photodiode
- APD avalanche photodiode
- photomultiplier tube a photomultiplier tube
- PMT charge injection device
- CID charge injection device
- CMOS based imager which transmits signals to readout device 28, such
- generator 30 excites electroluminescent layer 21 with a pulsed bias to
- time detection based on operating the TFELD in a pulsed mode.
- indicator agent is an intrinsic property, it offers the possibility of inherent
- the emission is delayed in time relative to the modulated excitation
- the vehicle is operated in time resolved, i.e., lifetime-based, mode.
- time resolved i.e., lifetime-based, mode.
- decay lifetime of the pulsed TFELD is at least one order of magnitude
- Figure 4 shows a schematic of the sensor of the invention in
- sensor layer 37 is exposed to medium 38 with analyte 39, which causes a
- PL 40 travels back d rough substrate 34, electroluminescent layer 31, and
- Electroluminescence 45 is emitted in pulsed mode from
- Sensor layer 46 is placed within a gas or liquid 47 with analyte, shown
- Photoluminescent emission 49 is reflected by mirror 50 back through
- An optical filter 52 is disposed between
- pulse generator 54 and pulse generator 55 are in electrical communication to permit
- EL 59 is emitted in a pulsed mode from layer 56 through substrate
- Probe or sensor layer 68 is
- An optical filter 64 is disposed between substrate 58 and photodetector 63 to filter
- oscilloscope 65 includes oscilloscope 65, computer 66, and pulse generator 67 in
- the system also includes an optional mirror
- Figure 7 shows a schematic of the probe or sensor of Figure 6.
- the schematic shows an electroluminescent layer 70 having transparent
- Electrodes 71 on one side of a transparent substrate 72.
- EL 73 is emitted
- Sensor layer 74 is disposed within gas or liquid 75 with analyte 76,
- the present invention also provides optical arrays of thin film
- indicator agents and matrix or other carrier materials may be any suitable indicator agents and matrix or other carrier materials, if present, may be any suitable indicator agents and matrix or other carrier materials, if present, may be any suitable indicator agents and matrix or other carrier materials, if present, may be any suitable indicator agents and matrix or other carrier materials, if present, may be any suitable indicator agents and matrix or other carrier materials, if present, may be any suitable indicator agents and matrix or other carrier materials, if present, may be
- a hazardous or toxic problem, or a clinical or environmental need may be detected by reaction with the array of
- sensor layers containing different indicator agents can be incorporated in
- an appropriate carrier or matrix e.g., polymers, sol-gels, and silicones, so
- Figure 8 shows a sensor array in a highly simplistic format.
- substantially rectangular supporting substrate 79 which can be flexible or
- surface 80 are a plurality of ti in film sensing layers 81, 82, 83, 84, 85 and
- each type of sensing layer is formulated
- the indicator In each sensing layer, the indicator
- agent in the absence of any analyte or mixture of ligands, is able to
- TFELDs 88, 89, and 90 On the opposite side of substate 87 there are TFELDs 88, 89, and 90, one TFELD
- Such sensor arrays are particularly well-suited for scaled up
- compositional gradients in the sensor units of an array can be induced in a
- indicator agents and carriers are used.
- the sensors can then be
- the TFELD-activated sensor array may be powered by any suitable
- in a fluid may be fabricated by electrically coupling the sensor leads of an
- the device measures changes in spectral response, wavelength,
- the device may include signal
- processing means in conjunction with a computer for qualitative and
- Such an array comprises at least ten
- Sensor measurements may be performed using the multisensor
- fluorescent light is then detected by, for example, a CCD array or camera.
- the CCD array or camera typically contains photosensitive elements
- the CCD array or camera may also contain one or more optical filters
- the detection may be carried out with a photographic color film which is processed later (e.g., for measuring the
- the optical sensing apparatus and instrumentation detects
- each sensing unit in the presence of and in the absence of a
- ligand or analyte of interest is collected by the CCD array or camera
- Wavelength range or Fluorescence emission
- the PL yield of tris(4,7-biphenyl- l,10-phenanthroline)Ru(II) chloride ("Ru(dpp)") is about 30% and it is
- Table 3 shows the quantum yields for a variety of fluorescent
- Ru(dpp) has the highest quantum yield of the
- the sensors of the invention can therefore be any sensors of the invention.
- Such reflected or emitted light energy is conveyed from the sensor layer
- sample can also be identified as a mixture of distinct entities or chemical
- a representative listing includes, for example, molecular oxygen, ionic species such as calcium and potassium, aromatic compounds
- hydrocarbon species esters, alcohols, amines, aldehydes, ketones,
- enzymes including, but not limited
- a dye and/or polymeric matrix surrounding a dye for example, a dye and/or polymeric matrix surrounding a dye
- analytes including, for example, ionic sensors, enzymatic
- sol-gel glasses include, for example, sol-gel glasses, polyacrylamide, PVC, and decyl
- Two general formats for polymeric matrix substances include a fully prepared polymer or copolymer, existing in bulk as a
- N0 2 " , and Cl " is that an ionophore (selective to the ion of interest), a
- chromoionophore generally a pH sensitive dye
- lipophilic additive generally a lipophilic additive
- a matrix e.g., PVC or decyl methacrylate.
- an ion of the analyte of interest is present it complexes with the
- range of the sensor unit can be tuned to the desired concentration range
- chromoionophore can be any suitable chromoionophore.
- the chromoionophore can be any suitable chromoionophore.
- a voltage sensitive dye e.g., Merocyanine 540, RH
- lactate is that the enzyme specific to the analyte is co-immobilized within
- the antibody is immobilized within a matrix or
- molecular beacon type optical sensors which can be used to detect DNA
- the operating principle is that a fluorophore and a quencher
- DNA strand containing d e fluorophore and the quencher is immobilized
- This example provides an all-organic miniature solid-state
- the sensor is a thin film of tris(4,7-biphenyl-
- porous sol-gel matrix the photoluminescence (PL) intensity and lifetime
- TFELD blue organic light
- OLED organic light emitting device
- hole-injecting anode was ⁇ 2000 A thick transparent 20 ⁇ /sq Applied
- ITO indium tin oxide
- TPD triphenyl diamine
- A1 2 0 3 buffer layer and d e electron-injecting Al metal layer The details on ITO cleaning and pretreatment as well as the preparation of the A1 2 0 3
- Electrodes were prepared as an array of round spots of 1.5 mm diameter;
- d e 5x5 cm substrate included about 200 OLEDs.
- sol-gel processing is an
- Ru(dpp) was purchased from GFS; all other reagents were
- silica sol was stirred for two
- sol-gel films were coated onto glass microscope cover-slips which had previously been
- sol-gel mix was pipetted onto the cover slip which was ti en spun at 1750
- the sensor signal was detected in the direct transmission
- OLEDs were operated in a pulsed mode with a pulse width of 1 - 7 ⁇ sec
- the EL an amplitude of 28 - 31 V, and a repetition rate of 13-120 kHz.
- the broad lamp emission was filtered by a 450 ⁇ 25nm band pass
- the dye-sol-gel mixture was deposited by a capillary pipette on
- the glass substrate also served as a
- OLED in air is shown in Figure 11. The objective was focused about
- the Blue OLED used was a small diameter
- bi-layer When excited by a train of rectangular voltage pulses, bi-layer
- organic OLEDs like those used in this experiment emit a bright light flash
- the Virgin Blue OLED exhibited a lifetime of 110 nanosec
- the long-lived tail was 2.3 microsec
- the long-lived component exhibited a lifetime of 1.9 microsec.
- the short-lived component of about 100 nanosec is probably associated
- the senor was produced using a spin-coating procedure.
- the sensor was
- the cover-slip was placed adjacent to the OLED glass substrate. All other
- the long-lived component exhibited a lifetime of 2 microsec.
- the short-lived component lifetime was about 290 nanosec.
- the sensor was applied by a capillary technique. A large-area
- the long-lived component exhibited a lifetime of 4.2 microsec.
- the short-lived component lifetime was about 270 nanosec.
- the short-lived component of 270 nanosec again can be
- the long-lived component is in the microsecond range, as
- the TFELD decay occurs in nanosecond scale (100-300
- peripheral apparatus and odier variations, alterations, substitutions or
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
KR1020017009250A KR20010101642A (en) | 1999-11-24 | 2000-11-21 | Optical sensors and arrays containing thin film electroluminescent devices |
AU27250/01A AU2725001A (en) | 1999-11-24 | 2000-11-21 | Optical sensors and arrays containing thin film electroluminescent devices |
EP00990188A EP1171764A1 (en) | 1999-11-24 | 2000-11-21 | Optical sensors and arrays containing thin film electroluminescent devices |
JP2001540355A JP2003515163A (en) | 1999-11-24 | 2000-11-21 | Optical sensor and array-containing thin film electroluminescent device |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US09/448,499 | 1999-11-24 | ||
US09/448,499 US6331438B1 (en) | 1999-11-24 | 1999-11-24 | Optical sensors and multisensor arrays containing thin film electroluminescent devices |
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EP (1) | EP1171764A1 (en) |
JP (1) | JP2003515163A (en) |
KR (1) | KR20010101642A (en) |
AU (1) | AU2725001A (en) |
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Also Published As
Publication number | Publication date |
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KR20010101642A (en) | 2001-11-14 |
US6331438B1 (en) | 2001-12-18 |
AU2725001A (en) | 2001-06-04 |
JP2003515163A (en) | 2003-04-22 |
EP1171764A1 (en) | 2002-01-16 |
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