CN102636471A - Miniflow control chip fluorescence detection system based on LED (light-emitting diode) excitation light source integrated with photonic crystal resonant cavity - Google Patents
Miniflow control chip fluorescence detection system based on LED (light-emitting diode) excitation light source integrated with photonic crystal resonant cavity Download PDFInfo
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- CN102636471A CN102636471A CN2012101269694A CN201210126969A CN102636471A CN 102636471 A CN102636471 A CN 102636471A CN 2012101269694 A CN2012101269694 A CN 2012101269694A CN 201210126969 A CN201210126969 A CN 201210126969A CN 102636471 A CN102636471 A CN 102636471A
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Abstract
The invention relates to a miniflow control chip fluorescence detection system based on LED (light emitting diode) excitation light source integrated with a photonic crystal resonant cavity. The detection system has a structure that a 2mum n type layer based on a III-V semiconductor material firstly grows on a substrate, then a reflect light layer grows on the substrate, an active layer based on the III-V semiconductor material grows, and finally a 200-300nm P type layer based on the III-V semiconductor material grows; and finally, a photon crystal resonant cavity pattern is sculptured on the P type layer through. According to the detection system, the sensitivity and distinguishability of the detection system can be improved through the generated narrow-band transmission spectra so as to induce fluorescence; and meanwhile, a photon forbidden band characteristic of the photon crystal resonant cavity is utilized, the side radiation of the excitation light source is effectively restrained, exciting light background noise is filtered, and the signal-to-noise ratio and noise proof property of the system are improved.
Description
Technical field
The invention belongs to biological sample (for example protein, DNA and antibody etc.) detection range; Relate to a kind of micro-fluidic chip fluorescence detecting system, can be applicable to disease treatment diagnosis and biomedical based on photonic crystal resonant cavity light emitting diode (LED) excitation source.
Background technology
Micro-fluidic chip plays a significant role in the research in fields such as genetic analysis, virus and Bacteria Detection, becomes one of main means that realize high flux " micro-full analytical system ".Though people obtain very big progress to the research of micro-fluidic chip in recent years, mainly still concentrate on development to the different microminiaturization of function, integrated micro-flow control chip itself.And it is backward relatively with the development of the supporting micro integrated detection system of micro-fluidic chip.Use in the current microfluidic analysis and comparatively generally be total to focusing laser-Induced Fluorescence Detection,, reach microminiaturized and integrated requirement far away though it has very high sensitivity.Although in the recent period big quantity research shows; Can be through integrated light-emitting diode (Light emitting diode in being total to focusing laser-induced fluorescence detection system; LED) and photodiode (Photodiode; PD) etc. method improves the micro integrated of system, but problem such as these researchs mostly are subject to the spectrum broad and the bigger system sensitivity that causes of side radiation of excitation source and resolution is low, signal to noise ratio (S/N ratio) is little.
Sensors and Actuators B, 2005 (106): 878-884, it has been reported PD has been integrated on the micro fluidic device, has set up chemical reaction detector, and has proved that PD has response characteristic preferably in the 600nm-700nm scope.Sensors and Actuators B, 2009 (140): 643-648, the micro-fluidic chip of the oxidation resistance screening that it develops PD integrated, and experiment has shown that PD has similar response characteristic with the photomultiplier of using always (PMT).Proc.SPIE 2005 (6036): 60361O-1, it adopts LED as excitation source in portable micro-fluidic detection system, with PD as detector.Yet they utilize LED or OLED as excitation source mostly, and the spectral bandwidth broad that therefore produces influences the sensitivity that system detects.Lab on a Chip, 2005 (5): 1041-1047 (2005), it is the microminiaturized fluorescence detecting system that excitation source has been set up micro-fluidic chip with OLED, utilizes homemade 300um optical filter to solve the problem of OLED emission spectrum broad simultaneously.Yet this method adopts the optical filter that separates, and makes the volume of detection system bigger than normal, and portability is lower.Optics Express; 2010 (18): 8781-8789; It has proposed a kind of based on vertical cavity surface emitting laser (Vertical-cavity-surface-emitting laser; VCSEL) the micro-fluidic chip fluorescent detection method of technology, the advantage of this method have also been realized the integrated of high precision and high index emission filter when being to reduce the width of emission spectrum.Yet VCSEL is too high with respect to complex manufacturing technology, the cost of LED and OLED, especially VCSEL side spontaneous radiation and the laser ground unrest that forms is difficult to filtering, therefore limited the detection sensitivity of total system.
Photonic crystal resonant cavity has the quality factor height, suppresses advantages such as the strong and volume of side spontaneous radiation ability is little, in micro-nano active optics devices field, important application prospects is arranged.Therefore, how integrated two-dimensional photonic crystal resonant cavity on the LED of micro-fluidic chip fluorescence detecting system excitation source makes it produce narrow emission spectrum, improves the sensitivity and the resolution of system; Utilize the forbidden photon band characteristic of photonic crystal resonant cavity simultaneously, effectively suppress the side radiation of LED, filtering exciting light ground unrest improves system signal noise ratio, is that wound of the present invention is ground motivation.
Summary of the invention
The present invention is directed to the problems referred to above, a kind of micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source is provided, this system has the advantages that size is little, highly sensitive, resolution is strong, accuracy rate is high, signal to noise ratio (S/N ratio) is good.
The present invention's technical scheme that adopts of dealing with problems is following:
A kind of micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source; The fluorescence induction excitation source of this system is to be made up of photonic crystal resonant cavity LED, and described LED is through on substrate, growing based on the n type layer of III-V family semiconductor material, reflector layer, based on the active layer of III-V family semiconductor material successively, forming based on the p type layer of III-V family semiconductor material; Integrated photon crystal resonator cavity on it makes its tool high quality factor and forbidden photon band, thereby realizes that arrowband live width and side radiation suppress the strong fluorescence induction excitation source of ability, and then improves resolution, sensitivity and the signal to noise ratio (S/N ratio) of system.
Described LED excitation source structure is through on substrate; Earlier about growth one deck 2 μ m based on the n type layer of III-V family semiconductor material; Regrowth one deck reflector layer; Grow based on the active layer of III-V family semiconductor material the p type layer that its secondary growth one deck 200-300nm is thick then based on III-V family semiconductor material.Through etching technics, etch the photonic crystal resonant cavity pattern at last in p type layer Window layer.
Described III-V family semiconductor material layer can be gallium phosphide (GaP), gallium aluminum arsenide (GaAlAs), gallium arsenide (GaAs), gallium nitride materials such as (GaN), and its inner structure has unilateral conduction
Described active layer can be the n InGaN/GaN quantum well or the quantum-dot structure in (n＞=4) individual cycle.
Described reflector layer can be metal level or distributed bragg reflector mirror (DBR), and metal level comprises metal levels such as Al, Ag, Au, Cu.
Described substrate can adopt crystalline material, organic material, and wherein crystalline material comprises silicon (Si), gallium arsenide (GaAs), indium phosphide (InP), sapphire (Al
2O
3) etc. Semiconductor substrate.
Described photonic crystal is rectangle, square, circular, oval figures, and the photonic crystal hole width is 20 nanometers to 10 micron, and height is in 60 nanometers to 10 centimetre.Periodically hole matrix can be realized through dry method or wet-etching technology; Like electron beam exposure (E-beam lithography), FIB exposure (Focus Ion Beam lithography) and reactive ion beam etching (RIBE) (Reactive Ion Etching; RIE) etc.; Be characterized in bottom flat, empty wall is smooth, and side view is not limit.
The preparation process of photonic crystal resonant cavity LED excitation source is on substrate, to prepare the semiconductor material base LED of III-V family through growth technique; On LED, prepare photonic crystal resonant cavity then through mask and etching technics.
Test macro of the present invention comprises according to compositions such as the flat excitation source of photonic crystal resonant cavity LED 14, exciting light filter plate 15, micro-fluidic chip 16, optical fiber 17, emission light optical filter 18, photomultiplier 19, high-voltage power supply 20 and computer control systems 21.
The invention has the beneficial effects as follows:
1, the present invention adopts photonic crystal resonant cavity LED as excitation source, replaces original semiconductor laser, and the size of micro-fluidic chip fluorescence detecting system is reduced.Simultaneously, needn't adopt the optical device of prism and lens combination, simplify detection system.
2, compare with existing micro-fluidic chip fluorescence detecting system, the present invention adopts photonic crystal resonant cavity that the side radiation of LED exciting light is restrained, and has improved the signal to noise ratio (S/N ratio) and the accuracy of system effectively.
3, because the photonic crystal resonant cavity that the present invention proposes has higher quality factor, the excitation spectrum live width of LED is narrowed down, effectively improve the resolution and the sensitivity of system.
Description of drawings
Fig. 1 is that photonic crystal resonant cavity LED excitation source is made schematic flow sheet.
Fig. 2 is a photonic crystal resonant cavity LED excitation source synoptic diagram.
Fig. 3 is based on the micro-fluidic chip fluorescence detecting system structural representation of photonic crystal resonant cavity LED excitation source.
Among the figure: 1 substrate; The semiconductor material n of 2III-V family type layer; 3 reflector layers;
4III-V family semiconductor material active layer; The semiconductor material p of 5III-V family type layer; 6 deposition mas;
7 photonic crystal resonant cavities; The 8ITO layer; 9p type electrode; 10n type electrode;
11 photonic crystal resonant cavity LED; 12 glass substrates; 13 cover glasses;
The flat light source of 14 photonic crystal resonant cavity LED; 15 exciting light filter plates; 16 micro-fluidic chips;
17 optical fiber; 18 emission light optical filters; 19 photomultipliers; 20 high-voltage power supplies; 21 computer control systems.
Embodiment
For making the content of technical scheme of the present invention more clear, be described in detail embodiment of the present invention below in conjunction with technical scheme and accompanying drawing.Film growth techniques wherein comprises: evaporation, sputter, metal organic chemical vapor deposition (MOCVD), molecular beam epitaxy (MBE), electron beam evaporation (E-beam evaporation) or liquid phase epitaxy common technologies such as (LPE).Mask process wherein comprise electron beam exposure (E-beam lithography, EBL), (Focus Ion Beam lithography FIBL) waits common technology for FIB exposure.Etching technics wherein comprises wet etching and dry etching, like acid system etching, electron beam lithography, focused-ion-beam lithography and reactive ion beam etching (RIBE) (Reactive Ion Etching, conventional process such as RIE).
At first; Adopt the MOCVD technology making the LED device on the substrate 1: the n type layer 2 about the growth one deck 2 μ m of elder generation based on III-V family semiconductor material; Regrowth one deck reflector layer 3 is grown based on the active layer 4 of III-V family semiconductor material then, the p type layer 5 based on III-V family semiconductor material that one deck 200-300nm that grows at last is thick; The epitaxial wafer growth is accomplished, shown in (a) in the accompanying drawing 1.Then, clean epitaxial wafer, carry out deposition mas 6, wherein 6 can be SiO
2Deng, shown in (b) in the accompanying drawing 1.
According to the result of Theoretical Calculation, the photonic crystal resonant cavity model of fill factor, curve factor and etching graphics request is satisfied in definition again, and makes public sample conversion to mask, shown in accompanying drawing 1 (c) through scan-type ion beam exposure or FIB.Wherein, Theoretical Calculation can adopt finite time-domain method of difference, finite element method scheduling algorithm.Through etching technics, preparation photonic crystal resonant cavity 7 on 5 materials is shown in (d) in the accompanying drawing 1.Then, remove mask 6, the cleaning of removing photoresist is shown like (e) in the accompanying drawing 1.Adopt the method for vacuum coating to make the thick ITO layer 8 of one deck 250-300nm at the photonic crystal resonant cavity upper surface again as current extending, shown in accompanying drawing 1 (f).Then, p type electrode 9 and following n type electrode 10 and annealing are gone up in preparation respectively, and 11 preparations of photonic crystal resonant cavity integrated LED are accomplished, shown in (g) in the accompanying drawing 1.
At last, photonic crystal resonant cavity integrated LED 11 is placed on the glass substrate 12, encapsulates, constitute the flat light source 14 of photonic crystal resonant cavity LED, shown in accompanying drawing 2 with cover glass 13.The volume size of light source 14 is close with micro-fluidic chip 16, is added in the voltage between p type electrode 9 and the n type electrode 10 through adjusting, and light source 14 sends the respective wavelength exciting light with certain intensity, is used to bring out fluorescence.Material through changing LED active layer 4 with mix, can make light source 11 with blue light, green glow, ruddiness and ultraviolet light.
As shown in Figure 3, test macro of the present invention mainly is made up of the flat excitation source of photonic crystal resonant cavity LED 14, exciting light filter plate 15, micro-fluidic chip 16, optical fiber 17, emission light optical filter 18, photomultiplier 19, high-voltage power supply 20 and computer control system 21 etc.Photonic crystal resonant cavity can effectively be restrained the side radiation of LED, and the high quality factor of photonic crystal resonant cavity also can effectively reduce the spectral width of exciting light simultaneously, improves the resolution and the sensitivity of system.The parasitic light that covers surveyed area in the exciting light that exciting light filter plate 15 can send excitation source 14 filters; The fluorescence signal that produces by exciting light 14 on the micro-fluidic chip 16; Be delivered to the emission light optical filter 18 of the other end through optical fiber 17; Filter the back and accepted amplification, transfer to computing machine 20 at last, write down the line data of going forward side by side by computing machine 21 and handle by photomultiplier 19.Sample cell on the micro-fluidic chip 16 is connected on the high-voltage power supply with the buffering solution pool, and high-voltage power supply 20 is connected with computing machine 21 simultaneously, is used for controlling electrophoresis sample introduction and lock out operation on the micro-fluidic chip 16.
In sum, photonic crystal resonant cavity LED excitation source provided by the invention has higher quality factor, so can obtain arrowband live width excitation spectrum, this characteristic can significantly improve the resolution and the sensitivity of micro-fluidic chip fluorescence detecting system.Simultaneously, the limit photosensitiveness that photonic crystal resonant cavity is good can effectively suppress the side radiation of LED, thereby improves the signal to noise ratio (S/N ratio) and the anti-interference of system.
The above is know-why and instantiation that the present invention uses, the equivalent transformation of doing according to conception of the present invention, as long as when the scheme that it used does not exceed spiritual that instructions and accompanying drawing contain yet, and all should be within the scope of the invention, explanation hereby.
Claims (8)
1. micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source; It is characterized in that; Based on photonic crystal resonant cavity LED excitation source is that photonic crystal resonant cavity is integrated in the excitation source on the LED; Its structure is the n type layer based on III-V family semiconductor material of elder generation's growth one deck 2 μ m on substrate; Regrowth one deck reflector layer, the one deck of growing then is based on the active layer of III-V family semiconductor material, the p type layer based on III-V family semiconductor material that one deck 200-300nm that grows at last is thick; Through etching technics, etch the photonic crystal resonant cavity pattern at last at p type layer.
2. the micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source according to claim 1; It is characterized in that described III-V family semiconductor material layer is gallium phosphide, gallium aluminum arsenide, gallium arsenide, the gallium nitride that inner structure has unilateral conduction.
3. the micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source according to claim 1 is characterized in that, described photonic crystal is a rectangle, square, circular, oval; The photonic crystal hole width is 20 nanometers to 10 micron, and height is in 60 nanometers to 10 centimetre.
4. the micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source according to claim 1 is characterized in that described active layer is the InGaN/GaN quantum well or the quantum-dot structure in n cycle, and wherein n is not less than 4.
5. according to claim 1 or 2 or 3 or 4 described micro-fluidic chip fluorescence detecting systems, it is characterized in that reflector layer is metal level or distributed bragg reflector mirror (DBR) based on photonic crystal resonant cavity LED excitation source.
6. according to claim 1 or 2 or 3 or 4 described micro-fluidic chip fluorescence detecting systems, it is characterized in that described substrate adopts crystalline material, organic material based on photonic crystal resonant cavity LED excitation source.
7. the micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source according to claim 5 is characterized in that the metal of metal level is meant Al, Ag, Au, Cu.
8. the micro-fluidic chip fluorescence detecting system based on photonic crystal resonant cavity LED excitation source according to claim 6 is characterized in that crystalline material comprises silicon, gallium arsenide, indium phosphide, sapphire.
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Cited By (5)
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| CN102879366A (en) * | 2012-09-21 | 2013-01-16 | 常州大学 | Liquid drop microfluidic system and method for detecting interaction between quantum dots and biomolecules |
| US9478713B2 (en) | 2014-05-27 | 2016-10-25 | Rohm And Haas Electronic Materials Llc | Nanostructure material methods and devices |
| CN106505076A (en) * | 2016-11-09 | 2017-03-15 | 太原理工大学 | Micrometre array LED preparation methoies |
| CN111785819A (en) * | 2020-06-29 | 2020-10-16 | 厦门大学 | GaN-based narrow-band emission resonant cavity light-emitting diode and manufacturing method thereof |
| DE102021212505A1 (en) | 2021-11-08 | 2023-05-11 | Robert Bosch Gesellschaft mit beschränkter Haftung | Optical device for exciting a sample, analyzer and method for exciting a sample |
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2012
- 2012-04-26 CN CN2012101269694A patent/CN102636471A/en active Pending
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Cited By (8)
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| CN102879366A (en) * | 2012-09-21 | 2013-01-16 | 常州大学 | Liquid drop microfluidic system and method for detecting interaction between quantum dots and biomolecules |
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| CN106505076A (en) * | 2016-11-09 | 2017-03-15 | 太原理工大学 | Micrometre array LED preparation methoies |
| CN106505076B (en) * | 2016-11-09 | 2018-07-31 | 太原理工大学 | Micrometre array LED preparation methods |
| CN111785819A (en) * | 2020-06-29 | 2020-10-16 | 厦门大学 | GaN-based narrow-band emission resonant cavity light-emitting diode and manufacturing method thereof |
| CN111785819B (en) * | 2020-06-29 | 2021-09-07 | 厦门大学 | GaN-based narrow-band emission resonant cavity light-emitting diode and manufacturing method thereof |
| DE102021212505A1 (en) | 2021-11-08 | 2023-05-11 | Robert Bosch Gesellschaft mit beschränkter Haftung | Optical device for exciting a sample, analyzer and method for exciting a sample |
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Application publication date: 20120815 |