CN104062249A - Method for detecting band gap changes of SiGe materials in electrochemical deposition process - Google Patents
Method for detecting band gap changes of SiGe materials in electrochemical deposition process Download PDFInfo
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- CN104062249A CN104062249A CN201410310069.4A CN201410310069A CN104062249A CN 104062249 A CN104062249 A CN 104062249A CN 201410310069 A CN201410310069 A CN 201410310069A CN 104062249 A CN104062249 A CN 104062249A
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Abstract
The invention provides a method for detecting band gap changes of SiGe materials in the electrochemical deposition process and belongs to the field of SiGe electro-deposition preparing methods. According to the method, a home position spectro-electro-chemistry technology is utilized, the changes of absorption spectrums of the SiGe materials in the deposition process are observed, and the deposition process and the SiGe band gap changes are analyzed. According to the method, the combination of an ionic liquid electro-deposition technology and a home position spectro-electro-chemistry method is utilized, environment-friendly ionic liquid [EMIm] Tf2N+GeCl4+SiC14 free of poison and pollution is used as an electrolytic solution, the electro-deposition step and measurement of the absorption spectrums are regulated and controlled, and the electro-deposition process of SiGe in the ionic liquid is represented in a home position mode; a semi-conductor which can absorb luminous energy strongly is utilized, and the changes of the absorption spectrums can reflect the speed of the electrochemical deposition process and the changes of band gaps in the deposition process. The detection method is simple in process, convenient to operate and easy to realize.
Description
Technical field
The invention belongs to SiGe electro-deposition preparation method field, be specifically related to the method for a kind of SiGe of detection material band gap variation in electrochemical deposition process.
Background technology
SiGe alloy is the novel semiconductor material rising in recent years, and it has the physical property of many uniquenesses, and it is widely used in electronics and opto-electronic semiconductor module.For example, can make heterojunction bipolar transistor (HBT), hetero junction field effect pipe (HFET), metal-oxide layer semiconductcor field effect transistor (MOSFET), heterojuction infrared detector (HIP), the multiple device such as low noise amplifier.SiGe also has very high refractive index, and its refractive index can regulate by changing the wherein content of germanium, and applicable preparation has the photonic crystal of complete photonic band gap.
At present, preparation SiGe material can be grown with multiple epitaxy method, as gas source molecular beam epitaxy (GSMBE), solid source molecular beam epitaxy (SSMBE) etc., although these methods can obtain the SiGe sediment of better quality, the deposition cost of common these class methods is higher and equipment manufacturing cost is expensive.And electrochemical deposition technique is a kind of new method of applicable preparation SiGe material.Electrochemical method is a kind of cryogenic technique, can suppress crystal growth (sedimental crystallite dimension is less), and by adjusting deposition voltage, current density and sedimentation time, changes composition and the thickness of deposition materials.Aqueous solution due to the separating out of hydrogen, cannot electro-deposition go out the semiconductor materials such as SiGe as electrolyte.And ionic liquid is as a kind of novel electrolytes, in galvanochemistry, there are a lot of advantages, as: 1. large 3. wide 4. required to electro-deposition semiconductor characteristics such as chloride favorable solubility of electrochemical window of the relatively low 2. conductivity of viscosity.So ionic liquid is applicable to the electro-deposition of SiGe material.
The existing research of ionic liquid electrodeposition preparation of SiGe, and people's research such as Salman is at [Py
isosorbide-5-Nitrae] Tf
2in N ionic liquid, in electro-deposition SiGe process, found interesting optical phenomena, analysis is because SiGe material causes the absorption of light in electrodeposition process.But utilize band gap variation in the electrodeposition process of research SiGe deposited film of absorption spectrum original position not have in addition relevant report.
Summary of the invention
The object of the invention is for the method for a kind of SiGe of detection material band gap variation in electrochemical deposition process is provided, the variation simple, that pass through absorption spectrum of this detection methodologies detects SiGe material band gap variation in electrochemical deposition process.
The method that the invention provides a kind of SiGe of detection material band gap variation in electrochemical deposition process, the method comprises:
Step 1: add GeCl in the two fluoroform sulfimide salt ion liquid of 1-ethyl-3-methylimidazole
4and SiCl
4, be mixed with electrolytic solution;
Step 2: using ITO substrate as working electrode, 99.999% platinum filament is as auxiliary electrode, and 99.999% filamentary silver is as contrast electrode, and utilizing electrolytic tank restriction SiGe depositional area is 0.3cm
2;
Step 3: electrolytic tank is connected on electrochemical workstation, and electrochemical workstation is connected with computing machine, and the electrolytic solution that step 1 is obtained joins in electrolytic tank, then electrolytic tank is fixed on support;
Step 4: wherein one of the optical fiber in optical fiber is connect to light source, collimating mirror is penetrated in other end access, reception collimating mirror of another root optical fiber, other end connects spectrometer, incident collimating mirror and reception collimating mirror are fixed on respectively the two ends up and down of electrolytic tank by support, spectrometer connects computing machine, for image data;
Step 5: open light source and spectrometer, open spectral measurement software, select absorption spectrum to measure, set delicate, scanning times 10 integral time 23720, smoothness 2, preserve successively again reference spectra and half-light spectrum deduction electrolytic solution back end, carry out the measurement of absorption spectrum;
Step 6: start electrochemical workstation, start Powersuite software, select the CyclicVoltammeter pattern in PowerCV to carry out cyclic voltammetry curve scanning, set successively working electrode, contrast electrode and electrolytic tank area;
Step 7: scanned after CV curve, select the Potential Step pattern in PowerCorr to carry out constant potential electro-deposition, set successively working electrode, contrast electrode and electrolytic tank area, deposition voltage is SiGe codeposition recovery voltage in CV curve, sedimentation time 1-15min, equilibration time 15s, often gathers spectroscopic data after one minute one time, by variation detection SiGe material band gap variation in electrochemical deposition process of spectroscopic data.
Preferably, the concentration of the electrolytic solution in described step 1 is 0.2mol/L.
Preferably, the two fluoroform sulfimide salt ion liquid of described 1-ethyl-3-methylimidazole before use should be in being full of the glove box of argon gas carries out the secondary processing of anhydrating, 100 ℃ of vacuum distillation 24h to it.
Preferably, described electrolytic tank is teflon electrolytic tank.
Preferably, in described step 4, incident collimating mirror is fixed on apart from 0.7cm place, electrolytic tank top, receives collimating mirror and is fixed on apart from 0.6cm place, electrolytic tank below.
Preferably, the measurement wavelength coverage 200-1100nm of described step 5.
Preferably, in described step 6, sweep limit-3V～3V is set, sweep speed 10mV/s, equilibration time 15s.
Beneficial effect of the present invention
The method that the invention provides a kind of SiGe of detection material band gap variation in electrochemical deposition process, the method is utilized In situ spectroscopic electrochemical techniques, observes the variation of SiGe material absorption spectrum in deposition process, analyzes deposition process and SiGe band gap variation; The present invention utilizes the combination of ionic liquid electrodeposition technology and In situ spectroscopic electrochemical process, uses green ionic liquid [EMIm] Tf of nontoxic pollution-free
2n+GeCl
4+ SiCl
4as electrolytic solution, regulation and control electrochemical deposition step and absorption spectrum are measured, the electrodeposition process of in-situ characterization SiGe in ionic liquid, this method has been utilized the absorption luminous energy that semiconductor can be strong, and the variation by absorption spectrum can reflect the variation of band gap in speed that electrochemical deposition process carries out, deposition process.This detection methodologies is simple, easy to operate, is easy to realize.
Accompanying drawing explanation
Fig. 1 is In situ spectroscopic electrochemical process device schematic diagram of the present invention;
Fig. 2 is 0.2mol/LSiCl of the present invention
4+ 0.2mol/LGeCl
4at [EMIm] Tf
2cyclic voltammetry curve in N ionic liquid;
Fig. 3 is [EMIm] Tf
2the absorption spectrogram of N ionic liquid;
Fig. 4 spectrogram of SiGe electrodeposition process that is the present invention under-2.7V voltage within the scope of 200-1100nm;
Fig. 5 spectrogram of SiGe electrodeposition process that is the present invention under-2.7V voltage within the scope of 300-600nm;
Fig. 6 is that the absorption spectra that deposits 1min in SiGe electrodeposition process of the present invention is done (α hv)
2the graph of a relation of～hv;
Fig. 7 is that the absorption spectra that deposits 15min in SiGe electrodeposition process of the present invention is done (α hv)
2the graph of a relation of～hv.
Wherein, 1, light source, 2, optical fiber, 3, working electrode, 4, electrolytic tank, 5, incident collimating mirror, 6, support, 7, spectrometer, 8, computing machine, 9, electrochemical workstation, 10, data line, 11, glove box, 12, receive collimating mirror.
Embodiment
The method that the invention provides a kind of SiGe of detection material band gap variation in electrochemical deposition process, the method comprises:
Step 1: at the two fluoroform sulfimide salt (EMImTf of 1-ethyl-3-methylimidazole
2n) in ionic liquid, add GeCl
4and SiCl
4, being mixed with electrolytic solution, the electrolytic solution being made into is standing 12-24h in glove box preferably, so that GeCl
4and SiCl
4in ionic liquid, can dissolve completely; The concentration of described electrolytic solution is preferably 0.2mol/L; The two fluoroform sulfimide salt ion liquid of described 1-ethyl-3-methylimidazole before use preferably should be in being full of the glove box of argon gas carries out the secondary processing of anhydrating, 100 ℃ of vacuum distillation 24h to it.
Step 2: using ITO substrate as working electrode, 99.999% platinum filament is as auxiliary electrode, and 99.999% filamentary silver is as contrast electrode, and utilizing electrolytic tank 4 restriction SiGe depositional areas is 0.3cm
2; Described ITO substrate in use, is preferably processed in the following manner: by ITO electro-conductive glass substrate, use successively each ultrasonic cleaning of acetone, methyl alcohol and ultrapure water 20-40min, after 100 ℃ of vacuum drying, clean 10-20min again with argon plasma; Described electrolytic tank 4 is teflon electrolytic tank;
Step 3: electrolytic tank 4 is connected on electrochemical workstation 9, and electrochemical workstation 9 is connected with computing machine 8, and the electrolytic solution that step 1 is obtained joins in electrolytic tank 4, then electrolytic tank 4 is fixed on support 6; Described electrochemical workstation 9 is preferably Princeton2273 electrochemical workstation;
Step 4: wherein one of the optical fiber in optical fiber 2 is connect to light source 1, collimating mirror 5 is penetrated in other end access, one of another root optical fiber receives collimating mirror 12, other end connects spectrometer, incident collimating mirror 5 and reception collimating mirror 12 are fixed on respectively the two ends up and down of electrolytic tank 4 by support 6, preferably incident collimating mirror 5 is fixed on apart from electrolytic tank 4 0.7cm places, top, receive collimating mirror 12 and are fixed on apart from electrolytic tank 4 0.6cm places, below, spectrometer 7 connects computing machine 8, for image data; Described light source 1 is preferably tungsten light source, and spectrometer 7 is preferably maya2000-Pro fiber spectrometer;
Step 5: open light source 1 and spectrometer 7, open spectral measurement software, selection absorption spectrum is measured, set microsecond integral time 23720, scanning times 10, smoothness 2, preserve successively again reference spectra and half-light spectrum deduction electrolytic solution back end, carry out the measurement of absorption spectrum, the measurement wavelength coverage of described step 5 is preferably 200-1100nm;
Step 6: start electrochemical workstation 9, start Powersuite software, select Cyclic Voltammeter (Ramp) pattern in PowerCV to carry out cyclic voltammetric (CV) curved scanning, setting successively working electrode is solid state electrode, contrast electrode is silver electrode, electrolytic tank area 0.3cm
2; Sweep limit-3V～3V is preferably set, sweep speed 1～10mV/s, equilibration time 15s;
Step 7: scanned after CV curve, selected the Potential Step pattern in PowerCorr to carry out constant potential electro-deposition, setting successively working electrode is solid state electrode, and contrast electrode is silver electrode, electrolytic tank area 0.3cm
2, deposition voltage is SiGe codeposition recovery voltage in CV curve, sedimentation time 1～15min, and equilibration time 15s, often gathers spectroscopic data after one minute one time, by variation detection SiGe material band gap variation in electrochemical deposition process of spectroscopic data.
After above-mentioned work completes, close light source, spectrometer, electrochemical workstation, disassemble electrolytic tank, after ito glass substrate is cleaned with absolute ethyl alcohol, preserve.
Fig. 1 is In situ spectroscopic electrochemical process device schematic diagram of the present invention, this device comprises lamp source 1, two optical fiber 2, working electrode 3, electrolytic tank 4, incident collimating mirror 5, support 6, spectrometer 7, computing machine 8, electrochemical workstation 9, data line 10, glove box 11 and accept collimating mirror 12, described working electrode 3 is arranged on 4 li, electrolytic tank, electrolytic tank 4 is fixed on support 6, electrolytic tank 4 is connected on electrochemical workstation 9, electrochemical workstation 9 is connected with computing machine 8, when work, three electrode (the working electrodes that electrochemical workstation 9 connects in electrolytic tank 4, auxiliary electrode, contrast electrode), by three-electrode system, control electrochemical process, the interior injection electrolytic solution of electrolytic tank 4, utilize electrochemical workstation 9 scan cycle volt-ampere (CV) curves, choose current potential and carry out constant potential electro-deposition,
Described optical fiber 2 is two, wherein one of an optical fiber connects light source 1, collimating mirror 5 is penetrated in other end access, one of another root optical fiber receives collimating mirror 12, and other end connects spectrometer, and incident collimating mirror 5 and reception collimating mirror 12 are fixed on respectively the two ends up and down of electrolytic tank 4 by support 6, preferably incident collimating mirror 5 is fixed on apart from electrolytic tank 4 0.7cm places, top, receive collimating mirror 12 and be fixed on apart from electrolytic tank 4 0.6cm places, below, spectrometer 7 connects computing machine 8, for image data; When work, first by light source 1, sending incident light is directional light through optical fiber 2 importing incident collimating mirrors 5 by light collimation, light exports to spectrometer 7 through entering reception collimating mirror 12 after sample via optical fiber 2, and spectrometer 7 passes through data line 10 by data input message collecting computer 8.
Below in conjunction with specific embodiment, the present invention is done to further detailed description.
Embodiment 1
1. by the two fluoroform sulfimide salt (EMImTf of 1-ethyl-3-methylimidazole
2n) ionic liquid carries out the secondary processing of anhydrating to it in being full of the glove box of argon gas, and 100 ℃ of vacuum distillation 24h, at [EMIm] Tf
2in N ionic liquid, add GeCl simultaneously
4and SiCl
4, be made into the electrolytic solution that concentration is 0.2mol/L.After mixing, the electrolytic solution being made into need to be in glove box standing 24h, make GeCl
4and SiCl
4in ionic liquid, dissolve completely;
2. by ITO electro-conductive glass substrate, use successively each ultrasonic cleaning of acetone, methyl alcohol and ultrapure water 20min, after 100 ℃ of vacuum drying, with argon plasma, clean 20min again, connecting electrode, using ITO substrate as working electrode, 99.999% platinum filament is as auxiliary electrode, and 99.999% filamentary silver is as contrast electrode, and utilizing teflon electrolytic tank 4 restriction depositional areas is 0.3cm
2;
3. electrolytic tank 4 is put into glove box 11 inside and outsides and connected Princeton2273 electrochemical workstation 9, Princeton2273 electrochemical workstation 9 connects computing machine 8, control galvanochemistry process, the electrolytic solution that step 1 is obtained is added dropwise in electrolytic tank 4, after electrolytic tank 4 is put on support 6;
4. wherein one of the optical fiber in optical fiber 2 is connect to tungsten light source 1, collimating mirror 5 is penetrated in other end access, one of another root optical fiber receives collimating mirror 12, other end connects maya2000-Pro fiber spectrometer, incident collimating mirror 5 is fixed on apart from electrolytic tank 4 0.7cm places, top, receive collimating mirror 12 and be fixed on apart from electrolytic tank 4 0.6cm places, below, maya2000-Pro fiber spectrometer 7 connects computing machine 8, for image data;
5. open tungsten light source 1 and maya2000-Pro fiber spectrometer 7, open spectral measurement software, selection absorption spectrum is measured, set delicate, scanning times 10 integral time 23720, smoothness 2, preserve successively again reference spectra and half-light spectrum deduction electrolytic solution back end, carry out the measurement of absorption spectrum, measure wavelength coverage 200-1100nm;
6. start Princeton2273 electrochemical workstation 9, start Powersuite software, select Cyclic Voltammeter (Ramp) pattern in PowerCV to carry out cyclic voltammetric (CV) curved scanning, setting successively working electrode is solid state electrode, contrast electrode is silver electrode, electrolytic tank area 0.3cm
2, sweep limit-3V～3V, sweep speed 1～10mV/s, equilibration time 15s;
7. scanned after CV curve, selected the Potential Step pattern in PowerCorr to carry out constant potential electro-deposition, setting successively working electrode is solid state electrode, and contrast electrode is silver electrode, electrolytic tank area 0.3cm
2deposition voltage is SiGe codeposition recovery voltage in CV curve, sedimentation time 1～15min, equilibration time 15s, in electrodeposition process, carry out the measurement of absorption spectrum, often gather after one minute spectroscopic data one time, by variation detection SiGe material band gap variation in electrochemical deposition process of spectroscopic data.
Fig. 2 is 0.2molSiCl of the present invention
4+ 0.2molGeCl
4at [EMIm] Tf
2cyclic voltammetry curve in N ionic liquid.As can be seen from the figure, the reduction peak in negative potential region is respectively Ge
4+→ Ge
2+with Ge
2+the reduction peak of → Ge, the acromion of-2.7V is corresponding to the codeposition reduction peak of SiGe.
Fig. 3 is the present invention [EMIm] Tf
2the absorption spectrogram of N ionic liquid.As can be seen from the figure there are two obvious absorption peaks at 400nm and 600nm left and right in ionic liquid, has two less absorption peaks near 900nm and 1000nm.
Fig. 4 spectrogram of SiGe electrodeposition process that is the present invention under-2.7V voltage within the scope of 200-1100nm; In figure, every curve represents the sedimentation time of a minute.As can be seen from the figure, the spectrogram of SiGe electrodeposition process is similar to Ge electro-deposition spectrogram, along with the increase absorption peak of sedimentation time strengthens gradually.
Fig. 5 spectrogram of SiGe electrodeposition process that is the present invention under-2.7V voltage within the scope of 300-600nm, as can be seen from the figure, dwindles after range of observation, has the red shift of 51nm between 368nm and 419nm.This red shift is because sedimental particle size growth occurs with gathering, and incipient stage particle size is little, due to quantum size effect, and band gap length; Along with particle size growth, band gap narrows down, and red shift appears in corresponding spectrum.
In order further solving, to be whether band gap changes, to depositing the absorption spectra of 1min and 15min in figure five, to do (α hv)
2after～hv graph of a relation, can obtain corresponding band gap variation, Fig. 6 is that the absorption spectra that deposits 1min in SiGe electrodeposition process of the present invention is done (α hv)
2the graph of a relation of～hv; Fig. 7 is that the absorption spectra that deposits 15min in SiGe electrodeposition process of the present invention is done (α hv)
2the graph of a relation of～hv; As can be seen from Figures 6 and 7, during deposition 1min, band gap is 2.65eV, and during deposition 15min, band gap is 1.86eV.Therefore,, along with the carrying out of deposition, sediment band gap has reduced 0.79eV.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
Above-mentioned explanation to the disclosed embodiments, makes professional and technical personnel in the field can realize or use the present invention.To the multiple modification of these embodiment, will be apparent for those skilled in the art, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (7)
1. a method that detects SiGe material band gap variation in electrochemical deposition process, is characterized in that, the method comprises:
Step 1: add GeCl in the two fluoroform sulfimide salt ion liquid of 1-ethyl-3-methylimidazole
4and SiCl
4, be mixed with electrolytic solution;
Step 2: using ITO substrate as working electrode, 99.999% platinum filament is as auxiliary electrode, and 99.999% filamentary silver is as contrast electrode, and utilizing electrolytic tank (4) restriction SiGe depositional area is 0.3cm
2;
Step 3: electrolytic tank (4) is connected on electrochemical workstation (9), electrochemical workstation (9) is connected with computing machine (8), the electrolytic solution that step 1 is obtained joins in electrolytic tank (4), then electrolytic tank (4) is fixed on support (6);
Step 4: wherein one of the optical fiber in optical fiber (2) is connect to light source (1), collimating mirror (5) is penetrated in other end access, one of another root optical fiber receives collimating mirror (12), other end connects spectrometer (7), incident collimating mirror (5) and reception collimating mirror (12) are fixed on respectively the two ends up and down of electrolytic tank (4) by support (6), spectrometer (7) connects computing machine (8), for image data;
Step 5: open light source (1) and spectrometer (7), open spectral measurement software, select absorption spectrum to measure, set delicate, scanning times 10 integral time 23720, smoothness 2, preserve successively again reference spectra and half-light spectrum deduction electrolytic solution back end, carry out the measurement of absorption spectrum;
Step 6: start electrochemical workstation (9), start Powersuite software, select the Cyclic Voltammeter pattern in PowerCV to carry out cyclic voltammetry curve scanning, set successively working electrode, contrast electrode and electrolytic tank (4) area;
Step 7: scanned after CV curve, select the Potential Step pattern in PowerCorr to carry out constant potential electro-deposition, set successively working electrode, contrast electrode and electrolytic tank area, deposition voltage is SiGe codeposition recovery voltage in CV curve, sedimentation time 1-15min, equilibration time 15s, often gathers spectroscopic data after one minute one time, by variation detection SiGe material band gap variation in electrochemical deposition process of spectroscopic data.
2. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, is characterized in that, the concentration of the electrolytic solution in described step 1 is 0.2mol/L.
3. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, it is characterized in that, the two fluoroform sulfimide salt ion liquid of described 1-ethyl-3-methylimidazole before use should be in being full of the glove box of argon gas carries out the secondary processing of anhydrating, 100 ℃ of vacuum distillation 24h to it.
4. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, is characterized in that, described electrolytic tank (4) is teflon electrolytic tank.
5. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, it is characterized in that, in described step 4, incident collimating mirror (5) is fixed on apart from 0.7cm place, electrolytic tank (4) top, receives collimating mirror (12) and is fixed on apart from 0.6cm place, electrolytic tank (4) below.
6. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, is characterized in that, the measurement wavelength coverage 200-1100nm of described step 5.
7. a kind of method that detects SiGe material band gap variation in electrochemical deposition process according to claim 1, is characterized in that, in described step 6, sweep limit-3V～3V is set, sweep speed 10mV/s, equilibration time 15s.
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| CN104988546A (en) * | 2015-07-28 | 2015-10-21 | 吉林师范大学 | Method for preparing germanium nano array by inducing ionic liquid electro-deposition with laser |
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| CN111118565A (en) * | 2019-12-25 | 2020-05-08 | 佛山科学技术学院 | Preparation method of Si-P film material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104988546A (en) * | 2015-07-28 | 2015-10-21 | 吉林师范大学 | Method for preparing germanium nano array by inducing ionic liquid electro-deposition with laser |
| CN105839146A (en) * | 2016-04-01 | 2016-08-10 | 宁夏邦鼎材料与环保科技有限公司 | Silicon-germanium solid solution and preparation method and application thereof |
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| CN111118565A (en) * | 2019-12-25 | 2020-05-08 | 佛山科学技术学院 | Preparation method of Si-P film material |
| CN111118565B (en) * | 2019-12-25 | 2022-03-22 | 佛山科学技术学院 | Preparation method of Si-P film material |
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| CN104062249B (en) | 2016-08-24 |
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