CN110734036A - On-chip spectrometer integrated on nanowire and preparation method of detector array thereof - Google Patents
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Abstract
The invention provides types of on-chip spectrometers integrated on a single semiconductor nanowire, which relate to the aspects of device design, device preparation methods, spectrometer working principles and the like, based on the physical properties of semiconductor nanowire materials and electrode metals, a Schottky junction type detector array integrated on the single semiconductor nanowire is reasonably designed, light to be detected is coupled into a semiconductor nanowire waveguide with high reflectivity through a designed coupler, the high sensitivity of a Schottky diode and the enhanced light and matter action of the waveguide jointly determine that the device has high photoelectric detection rate, and weak light signals can be detected, so that a chip-integrated micro spectrometer is realized.
Description
Technical Field
The invention relates to semiconductor nano materials, micro-nano optics, electrical elements and systems, in particular to a micro-chip integrated high-detection-rate spectrometer and a detection array preparation method.
Background
The micro spectral analysis chip belongs to the international frontier research field, the research on the field is gradually deepened at present, the realization of wide spectral wavelength resolution, the exploration of new application and the research on new physical effects become the current key points, Naure 523,67 (2015) reports new methods for manufacturing a high-resolution spectrometer based on colloidal quantum dot materials in cooperation of Bajie and M.Bandi, quantum dots with different forbidden bandwidths are adopted as filters to realize spectral analysis, recently Science 365, 1017 + 1020 (2019) reports that Hasan Tawque at Cambridge university is integrated in a single-root micro-scale-nano-wire spectrometer, adopts a light guide type detection principle, realizes the intelligent spectrum detection principle by a back-illumination mode, and people have intelligent spectrum analysis, such as the development of aerospace devices, the development of aerospace devices and the like.
Although the existing micro spectrometer makes great progress, the existing micro spectrometer has various limitations that the original framework is not broken through by adopting the micro grating essentially, the space cannot be compact, the methods for realizing the light splitting technology by adopting the photonic crystal, the metamaterial or the plasmon have higher cost and narrower distinguishable spectrum range, light to be detected reaches the surface of a detector in a back incidence mode, the original spectrum is easy to distort, and most importantly, the existing micro spectrum system is difficult to realize high detection rate, so that on-chip spectrum analysis, particularly weak light detection, is greatly challenged.
Disclosure of Invention
The invention aims to provide miniature high-detectivity on-chip spectrometers integrated on single semiconductor nanowires with gradually-changed band gaps, which comprise a method for preparing a Schottky diode detector array integrated on the single semiconductor nanowire and a method for reconstructing the spectrum of a light source to be measured on a chip by a waveguide coupling method.
The invention discloses types of on-chip spectrometers integrated on nanowires, which comprise Schottky detector arrays integrated on single semiconductor nanowires with gradually changed band gaps and used for realizing microchip integrated spectrum detection, wherein light to be detected in the Schottky detector arrays enters from ports of the semiconductor nanowires with gradually changed band gaps and is transmitted and detected along the nanowires in a waveguide coupling mode, the diameters of the semiconductor nanowires with gradually changed band gaps are 100-1000nm, and the lengths of the semiconductor nanowires with gradually changed band gaps are from several micrometers to hundreds of micrometers.
According to the on-chip spectrometer integrated with the nanowire, which is defined by steps, the semiconductor nanowire with the gradually-changed band gap is made of high-reflectivity band gap gradually-changed materials such as CdSxSe1-x, ZnCdSxSe1-x, SiGeSn or nanowires with the gradually-changed band gaps of three groups and five groups.
In the above-mentioned on-chip spectrometer integrated on a nanowire, the light to be detected is coupled into the semiconductor nanowire through the waveguide coupler, and the light to be detected is incident from the wide bandgap end of the semiconductor nanowire; the waveguide coupler is a waveguide structure which couples an on-chip or external light source into the detector through a grating waveguide or an optical fiber waveguide, the Schottky detector arrays are all Schottky diodes, the Schottky diodes are arranged along the length direction of the semiconductor nanowires with gradually changed band gaps, and the arrangement direction of the Schottky diodes is perpendicular to the semiconductor nanowires with gradually changed band gaps.
A method for preparing a Schottky detector array for a nanowire-integrated on-chip spectrometer, comprising the steps of:
1) in a tubular furnace, gold particles are used as a catalyst, and a method of introducing a moving source by using a gas-liquid-solid (VLS) is adopted to prepare a nanowire with a gradually changed CdSSe band gap under the conditions of 800-900 ℃ vapor pressure of 100-500 mba;
2) transferring the nanowires onto a silicon wafer or a glass sheet in a mechanical friction mode, selecting the nanowires with the morphology and the luminous efficiency meeting the requirements under a fluorescence microscope, and then picking the target nanowires onto the silicon wafer with silica with the thickness of 285nm through a transfer platform with tapered optical fibers;
3) moving a series of electronic etching thin films with the thickness of more than 200 nmPMMA (nanometer plasma display panel) onto the nanowire substrate to realize covering of photoresist;
4) and obtaining a template of the electrode by using an electron beam exposure technology, wherein the electron beam current of the electron beam exposure is 10 na-300, the dose is 1200 mu C, the electrode spacing is 1 mu m, the duty ratio is 1:1, and then obtaining the metal electrode by using an electron beam evaporation technology.
Schottky detector array preparation method, the step of covering photoresist in the step (3) comprises the steps of cleaning a substrate, spin-coating a PMMA solution with the concentration of 1-10%, the spin-coating rotation speed is 1000-.
In the method for manufacturing the schottky detector array, the metal electrode and the nanowire form a back-to-back schottky junction, or an asymmetric electrode is adopted to form a schottky junction; the metal electrode adopts titanium, gold, platinum, aluminum, silver, palladium or a thin graphene film as an electrode.
, the invention also discloses the application of Schottky detector arrays for the spectral analysis of molecular, atomic, cellular and crystalline materials on a chip.
The invention has the beneficial effects that the semiconductor nanowires with gradually changed band gaps are used as the main body material and the waveguide of the detector, the mature modern micromachining technology is utilized to prepare the device, the on-chip spectrometer has the outstanding characteristics of high detection rate and a direct incidence mode of a light source to be detected, and has important functions of weak light spectrum analysis and in-situ detection on a chip, which are functions difficult to realize by other micro spectrometers.
Drawings
FIG. 1 is a schematic diagram of a waveguide mode spectrum detection
FIG. 2 is a schematic diagram of a process for fabricating a device of the present invention.
FIG. 3, (a) optical microscope photograph of an array of devices; (b) the absorption spectrum of the waveguide mode is compared with the absorption spectrum of the normal incidence.
Fig. 4, ohmic contact device versus schottky device: (a) comparing the noise performance; (b) light dark current contrast; (c) contrast of light dark current with time; (d) device statistics of dark current over time.
FIG. 5 is a spectrum test resolution test using the spectrometer on chip of the present invention.
FIG. 6 is a reconstruction of a continuum of light spectra obtained using the on-chip spectrometer of the present invention.
FIG. 7 is a reconstruction of an on-chip spectrum obtained by the on-chip spectrometer of the present invention.
Fig. 8 is a schematic structural diagram of fig. 1.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
This embodiment proposes methods for manufacturing a schottky detector array for a spectrometer integrated on a nanowire chip, comprising the following steps:
1) preparing a CdSSe band gap gradient nanowire 1 by introducing a moving source through a vapor-liquid-solid (VLS) method under the condition of 860 ℃ vapor pressure 300 mba by taking gold particles as a catalyst in a tubular furnace;
2) transferring the nanowires onto a silicon wafer or a glass sheet in a mechanical friction mode, selecting the nanowires with good appearance and luminescence under a fluorescence microscope, and then picking the target nanowires onto the silicon wafer with silica with the thickness of 285nm through a transfer platform with a tapered optical fiber;
3) moving a series of electronic etching thin films with the thickness of more than 200 nmPMMA (nanometer plasma display panel) onto the nanowire substrate to realize covering of photoresist;
4) and obtaining a template of the electrode by using an electron beam exposure technology, wherein the electron beam current of the electron beam exposure is 10 na-300, the dose is 1200 mu C, the electrode spacing is 1 mu m, the duty ratio is 1:1, and then obtaining the metal electrode by using an electron beam evaporation technology.
As shown in FIG. 1, the on-chip spectrometer used in the example comprises a semiconductor nanowire 1 with a gradually-changed band gap and a Schottky diode array 2 which are arranged on a silicon oxide substrate 5, wherein metal and nanowire contacts are Schottky contacts, the nanowire serves as a waveguide, light 3 to be detected in the Schottky detector array enters from the port of the semiconductor nanowire with the gradually-changed band gap and is transmitted and detected along the nanowire through a waveguide coupler 4, a filter 6 is arranged between the waveguide coupler and the semiconductor nanowire, and the filter 6 of an imaging optical path adopts a filter with a low pass of 500nm and mainly has the function of filtering out an exciting light signal.
And (3) placing the nanowire sample obtained in the step (2) under an optical fluorescence microscope, selecting high-quality nanowires, and transferring the nanowires to a silica substrate with the thickness of 280nm by using a three-dimensional adjusting frame and a self-made fiber needle. And (3) transferring the transferred nanowire sample obtained in the step (3) to PMMA4 by using a transfer method and cover the nanowire, and then making an electrode layout by using an EBPG5200 electron beam exposure system, wherein the beam current used in the process is 10nA, and the dose is 1200 mu C. And (4) preparing a Ti (1nm)/Au (50nm) electrode by adopting an EBE (electron beam emitter) method and performing lift-off on the patterned electrode obtained in the step (4). The device obtained in step 5 was placed under a microscope under blue LED illumination, and the resulting photomicrograph is shown in fig. 3 (a), where the color lines from green to red can be seen.
The specific method for growing the semiconductor nanowire with the gradually-changed band gap disclosed in this embodiment is to use a method of introducing a moving source and a substrate during a vapor-liquid-solid (VLS) growth process, use gold particles as a catalyst, and use a method of introducing a moving source by a vapor-liquid-solid (VLS) under a vapor pressure of 860 ° 300 mba to prepare a nanowire with a gradually-changed band gap of CdSSe, and fig. 1 shows a photograph of the grown CdSSe nanowire with a gradually-changed band gap and a fluorescence microscope. The same method can also be used for growing nanowires such as CdSSe and ZnCdSSe, and SiGeSn can be realized by adopting a method of metal-induced plasma enhanced chemical vapor deposition.
The technology for transferring the nanowires to the target substrate in this embodiment is to transfer the nanowires 1 to substrates 5 by mechanical friction, where the substrates are selected from quartz glass or silicon wafers, then find the high-quality nanowires with gradually-changed band gaps under a fluorescence microscope, pick the selected nanowires onto the target substrate by a thinned optical fiber under the microscope, or stick the nanowires onto the target substrate by a PVA or PDMS method.
The key technology for preparing the single nanowire schottky diode array required to be prepared in the embodiment comprises the steps of selecting a proper device structure through physical analysis of a metal semiconductor, then realizing patterning of the device through an electron beam etching method, and then depositing electrode metal through an electron beam evaporation method. Fig. 2 is a single nanowire array implemented in a laboratory and a fluorescence diagram thereof.
The photoresist related in the embodiment is PMMA4, and the photoresist is covered by a spin coating or transferring method; the photoresist transfer step comprises: cleaning a substrate, wherein the substrate is silicon dioxide, silicon or mica; spin-coating a substrate with 1-10% PMMA solution at a spin-coating speed of 1000-4000 rpm for 30-60s, and drying; separating the substrate and the PMMA film by using etching liquid, wherein the etching liquid is sodium hydroxide solution, hydrofluoric acid solution or water; fishing out the PMMA film by using a support frame, and drying at the temperature of 50 ℃ for 5-10 min; covering the target substrate with the support frame, and heating at 110-; and separating the support frame, and finishing the transfer of the PMMA film. The asymmetric electrode can adopt an alignment technology, and flexible conductive films such as thin graphene and the like are used as electrodes, and an electrode pattern is etched by a reactive ion etching process.
The light to be measured needs to be coupled and incident to be detected from a forbidden band end of the semiconductor nanowire, the light to be measured can directly irradiate a wide band gap end of the semiconductor nanowire and can also be coupled into the nanowire through an optical fiber coupler, the electrodes are connected with an external circuit through a wire-bonding method by devices, the light current of each pair of devices is measured, the spectrum reconstruction technology comprises matrixes of devices of a single semiconductor nanowire device array and the light current corresponding to a light source to be measured, and the spectrum of the light source to be measured is obtained through a spectrum reconstruction formula.
In the embodiment, a detected light source is coupled into the nanowire through a waveguide mode, and in the embodiment, the absorption curves of devices are matched with the vertical incidence and the waveguide mode incidence of the light source, so that the detection effect of the device is samples, the light source used in the embodiment is provided by a super-continuum spectrum laser (model SC-Pro-7), and the laser spectrum is continuously adjustable (the wavelength adjustable range is 400-2000 nm).
Example 1 test of Low noise characteristics
In this example, different electrode contacts using the same nanowire are compared: the weak signal characteristics of the two devices, schottky contact and ohmic contact, compare the noise of the two devices as shown in fig. 4 (a), and it can be seen that the device noise of the schottky contact is 6 orders of magnitude lower than that of the ohmic contact; FIGS. 4 (b) and (c) show a comparison of dark current and photocurrent for weak signals for two devices, particularly the 150 pA photocurrent obtained with the Schottky junction detector of FIG. 4 (c) when using a 532 nm laser of 8.8 nW as the probe light, and remained stable over time, as opposed to the effective photocurrent obtained with the ohmic contact detector which was essentially ineffective and fluctuated significantly over time; in the device array, the dark current stability of the devices with ohmic contacts and the devices with schottky contacts is randomly sampled and tested, and statistics are carried out as shown in fig. 4 (d), the dark current of the devices with ohmic contacts and the dark current of the devices with ohmic contacts fluctuate and change along with time, and the devices with schottky contacts have small difference and good stability. The prepared Schottky basic detector array based on the nano-wires shows that the device array with the Schottky contact has good stability, low noise and obvious advantages in weak light detection, especially on-chip spectrum analysis.
Example 2 micro spectrometer resolution test
In the resolution test of the embodiment, a supercontinuum laser generates two laser lines, the two laser lines are simultaneously focused on the broadband end of a nanowire through an optical microscope, the diameter of a light spot is smaller than 1 micron, the size of photocurrent generated by each pair of electrodes is respectively tested, the spectral shapes of the two spectra are reconstructed through a formula by combining the photoresponse curves of all devices, and then the peak values of the two laser wavelengths are continuously reduced until the two laser wavelengths are just distinguished; as shown in fig. 5, the spectral shape of the commercial spectrometer and our mini spectrometer is compared by changing the interval of the two incident laser wavelengths, and it can be seen that the device in this example can distinguish 10 nm at the minimum; the resolution also depends on the gradient rate of the forbidden band of the nanowire itself in the axial direction and the electrode density. Resolution of 10 nm has met many requirements such as portable biomolecule spectroscopic analysis and biomolecule imaging and smart device applications.
Example 3 continuous Spectroscopy testing
In this embodiment, a super-continuum spectrum laser is used to provide a white light source, the white light source is focused on the forbidden bandwidth end of a nanowire device through a microscope, the photocurrent of each pair of electrodes in the device array is tested, the spectral shape of a spectrum to be measured is reconstructed through a formula by combining the photoresponse curve of each device, as shown in fig. 6, the spectral shape of the white light laser measured by a commercial spectrometer is compared with the spectral shape obtained by reconstructing the micro spectrometer, the visible matching degree is very high, and the good spectral analysis function of the nanowire spectrometer is fully demonstrated, so that the nano-line spectrometer can be applied to on-chip spectral analysis.
Example 4 on-chip Spectroscopy testing
In this example, the on-chip spectrometer of the present invention is used to test an on-chip light source, as shown in fig. 7, the embedded graph is a test schematic diagram, light-emitting nanowires are picked up by an optical fiber, the head and the ground are aligned with the spectrometer nanowires, laser light is irradiated on the to-be-tested nanowires, nanowire fluorescence enters the spectrometer through the waveguide coupling of the nanowires themselves, a photocurrent signal of a spectrometer device is tested, a spectral signal of the to-be-tested light source is obtained by a reconstruction method as shown in fig. 7, and it can be seen that a spectrum tested by using the on-chip spectrometer of the present invention.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.
Claims (10)
1. An on-chip spectrometer integrated on a nanowire, comprising: the Schottky detector array comprises a Schottky detector array integrated on a single semiconductor nanowire with gradually changed band gap, and is used for realizing the spectrum detection of microchip integration; light to be detected in the Schottky detector array enters from the port of the semiconductor nanowire with the gradually changed band gap and is transmitted and detected along the nanowire in a waveguide coupling mode; the diameter of the semiconductor nanowire with the gradually changed band gap is 100-1000nm, and the length of the semiconductor nanowire is from several micrometers to several hundred micrometers.
2. The nanowire-integrated on-chip spectrometer of claim 1, wherein: the semiconductor nanowire with the gradually-changed band gap has the following high-reflectivity band gap gradually-changed materials: CdSxSe1-x, ZnCdSxSe1-x, SiGeSn, or three-five group nanowires with gradually changed band gaps.
3. The nanowire-integrated on-chip spectrometer of claim 1, wherein: the light to be detected is coupled into the semiconductor nanowire through the waveguide coupler, and the light to be detected is incident from the wide forbidden band end of the semiconductor nanowire.
4. The nanowire-integrated on-chip spectrometer of claim 3, wherein: the waveguide coupler adopts grating waveguide or fiber waveguide to couple on-chip or external light source into the waveguide structure of the detector.
5. The nanowire-integrated on-chip spectrometer of claim 1, wherein: the Schottky detector arrays are all Schottky diodes, the Schottky diodes are arranged along the length direction of the semiconductor nanowires with gradually changed band gaps, and the arrangement direction of the Schottky diodes is perpendicular to the semiconductor nanowires with gradually changed band gaps.
6. A method of fabricating a schottky detector array as described in claim 1, comprising the steps of:
1) in a tubular furnace, gold particles are used as a catalyst, and a method of introducing a moving source by using a gas-liquid-solid (VLS) is adopted to prepare a nanowire with a gradually changed CdSSe band gap under the conditions of 800-900 ℃ vapor pressure of 100-500 mba;
2) transferring the nanowires onto a silicon wafer or a glass sheet in a mechanical friction mode, selecting the nanowires with the morphology and the luminous efficiency meeting the requirements under a fluorescence microscope, and then picking the target nanowires onto the silicon wafer with silica with the thickness of 285nm through a transfer platform with tapered optical fibers;
3) moving a series of electronic etching thin films with the thickness of more than 200 nmPMMA (nanometer plasma display panel) onto the nanowire substrate to realize covering of photoresist;
4) and obtaining a template of the electrode by using an electron beam exposure technology, wherein the electron beam current of the electron beam exposure is 10 na-300, the dose is 1200 mu C, the electrode spacing is 1 mu m, the duty ratio is 1:1, and then obtaining the metal electrode by using an electron beam evaporation technology.
7. The method of fabricating a schottky detector array as described in claim 6 wherein: the step of covering the photoresist in the step (3) comprises the following steps: cleaning the substrate; spin-coating a substrate with 1-10% PMMA solution at a spin-coating speed of 1000-4000 rpm for 30-60s, and drying; separating the substrate and the PMMA film by using etching liquid, wherein the etching liquid is sodium hydroxide solution, hydrofluoric acid solution or water; fishing out the PMMA film by using a support frame, and drying at the temperature of 50 ℃ for 5-10 min; covering the target substrate with the support frame, and heating at 110-; and separating the support frame, and finishing the transfer of the PMMA film.
8. The method of fabricating a schottky detector array as described in claim 6 wherein: the metal electrode and the nanowire form a back-to-back Schottky junction, or an asymmetric electrode is adopted to form the Schottky junction.
9. The method of fabricating a schottky detector array as described in claim 8 wherein: the metal electrode adopts titanium, gold, platinum, aluminum, silver, palladium or a thin graphene film as an electrode.
10. The use of a schottky detector array as in claim 6 wherein: for spectroscopic analysis of molecular, atomic, cellular and crystalline materials on a chip.
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