CN102263373B - Surface-textured-zinc oxide (ZnO)-film-based electrically pumped random laser and preparation method - Google Patents

Surface-textured-zinc oxide (ZnO)-film-based electrically pumped random laser and preparation method Download PDF

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CN102263373B
CN102263373B CN 201110172770 CN201110172770A CN102263373B CN 102263373 B CN102263373 B CN 102263373B CN 201110172770 CN201110172770 CN 201110172770 CN 201110172770 A CN201110172770 A CN 201110172770A CN 102263373 B CN102263373 B CN 102263373B
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random laser
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zno film
texturing
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CN102263373A (en
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马向阳
李云鹏
杨德仁
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Zhejiang University ZJU
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Abstract

The invention discloses a surface-textured-zinc oxide (ZnO)-film-based electrically pumped random laser and a preparation method. The method comprises the following steps of: depositing a ZnO thin film on the front of a substrate, arranging the substrate in a hydrochloric acid for corrosion, taking the substrate out for washing, depositing a silicon dioxide (SiO2) thin film on the ZnO thin film and depositing an Au electrode on the back of the substrate and the SiO2 thin film. Compared with the conventional electrically pumped random laser, the electrically pumped random laser prepared by the method remarkably reduces threshold current, and embodiments 1 and 2 show that the threshold current is reduced for about a half.

Description

Electric pumping random laser and preparation method based on the surface-texturing ZnO film
Technical field
The present invention relates to field of optoelectronic devices, relate in particular to a kind of electric pumping random laser based on the surface-texturing ZnO film and preparation method thereof.
Background technology
Sharp penetrating is a kind of luminescence phenomenon that results from the random media at random.Different from conventional laser is, swash at random the generation of penetrating and need not to prepare accurate resonant cavity, and the light emission direction random distribution, its unique performance has potential using value at plane demonstration, biological medicine, military aspect.The ZnO material is considered to prepare the ideal material of ultraviolet accidental laser owing to have higher optical gain and stronger light scattering ability.
2007, horse is waited on the sunny side and has utilized Metal-oxide-semicondutor (MOS) structure to realize the electric pumping random laser (X.Y.Ma of ZnO polycrystal film, P.L.Chen, D.S.Li, Y.Y.Zhang, D.R.Yang, Electrically pumped ZnO film ultraviolet random lasers on silicon substrate.Appl.Phys.Lett.91,2007,251109).In this report, the threshold current of Random Laser is about 70mA, and the thermal effect that too high electric current produces can affect performance of devices, and the integrated difficulty of device is strengthened.Therefore, reduce threshold current and become the primary goal that device performance is optimized.
Summary of the invention
The invention provides a kind of preparation method of the electric pumping random laser based on surface-texturing (surface texture) ZnO film, solved device and swashed at random the too high problem of threshold current of penetrating.
A kind of preparation method of electric pumping random laser comprises:
At substrate face deposition ZnO film, place hydrochloric acid to corrode, taking-up cleans up, and deposits SiO at ZnO film 2Film is at substrate back and SiO 2Thin film deposition Au electrode.
Deposition ZnO film, Au electrode all can adopt the method for dc reactive sputtering, deposit SiO at ZnO film 2Film can adopt sol-gel process.
Surface-texturing of the present invention refers to that the ZnO film surface forms the pattern that height rises and falls behind hcl corrosion.
Preferably, the concentration of described hydrochloric acid is 0.005~0.03mol/L, and described corrosion temperature is 20~50 ℃, and the time is 3~15 seconds.
Preferably, behind the described substrate face deposition ZnO film, prior to heat treated under the oxygen atmosphere, then place hydrochloric acid to corrode, to improve the crystalline quality of ZnO film, the heat treated temperature is preferably 600~800 ℃, and the time is preferably 1~3 hour.
The electric pumping random laser that the present invention also provides above-mentioned preparation method to make.
Beneficial effect of the present invention is: with respect to traditional electric pumping random laser, the threshold current of the electric pumping random laser that the inventive method makes significantly reduces, and can find out that from embodiment 1 and embodiment 2 threshold current has descended about half.
Description of drawings
Fig. 1 is the structural representation of electric pumping random laser of the present invention;
Fig. 2 is the stereoscan photograph of the ZnO film processed without surface-texturing among the embodiment 1;
Fig. 3 is the stereoscan photograph of ZnO film after surface-texturing is processed among the embodiment 1;
Fig. 4 is the luminous spectrum of electric pumping random laser under different electric currents of the ZnO film after surface-texturing is processed among the embodiment 1;
Fig. 5 is the luminous spectrum of electric pumping random laser under different electric currents of the ZnO film processed without surface-texturing among the embodiment 1;
Fig. 6 is the Output optical power curve of two kinds of electric pumping random lasers under different electric currents among the embodiment 1, curve 1 is corresponding to the electric pumping random laser of the ZnO film after processing through surface-texturing, and curve 2 is corresponding to the electric pumping random laser of the ZnO film of processing without surface-texturing;
Fig. 7 is the stereoscan photograph of ZnO film after surface-texturing is processed among the embodiment 2;
Fig. 8 is the luminous spectrum of electric pumping random laser under different electric currents of the ZnO film after surface-texturing is processed among the embodiment 2.
Embodiment
As shown in Figure 1: a kind of electric pumping random laser, comprise the substrate 1 of being made by the N-type silicon chip, substrate face deposits luminescent layer 2, and this luminescent layer 2 is the surface-texturing ZnO film, and luminescent layer deposits barrier layer 3, and barrier layer 3 is SiO 2Film, barrier layer 3 and substrate 1 back side deposit respectively Au electrode 4 and the gold thin film 5 that thickness is about 20nm and 100nm, as the electrode of device.This device can prepare by the following method.
Embodiment 1
1) getting resistivity is that 0.005 ohmcm, size are 15 * 15mm 2, thickness is two N-type<100 of 675 microns silicon chip, put into the reative cell of dc reactive sputtering device after the cleaning, the reative cell vacuum is evacuated to 5 * 10 -3Pa; Utilize the method for dc reactive sputtering to deposit the thick ZnO film of about 160nm at silicon chip, when sputter, adopt simple metal Zn target, 300 ℃ of underlayer temperatures, sputtering power 100W, pass to O 2With Ar mist, O 2With the flow-rate ratio of Ar be 1: 2, operating pressure is 8Pa; Under oxygen atmosphere, 700 ℃ temperature, heat-treated 2 hours;
2) adopting concentration is the dilute hydrochloric acid solution of 0.02mol/L, under 40 ℃ to the ZnO film corrosion on a slice silicon chip wherein 10 seconds, next with deionized water residual HCl solution is rinsed well;
3) utilize sol-gel process to deposit SiO at above-mentioned two kinds of ZnO films 2Film, concrete steps are as follows: configuration tetraethoxysilane (TEOS): the precursor solution of ethanol (EtOH)=1: 10 (mol ratio), and the HCl that adds trace stirs after 2 hours, as SiO as catalyst 2Precursor sol.At the speed spin coating one deck SiO of above-mentioned two kinds of ZnO films with 3000 revolutions per seconds 2The precursor sol film, then 100 ℃ of lower oven dry 20 minutes, in air, formed SiO in 1 hour in 550 ℃ of heat treatments at last 2Film;
4) at SiO 2The thick translucent Au electrode of the about 20nm of sputter on the film, at the thick Au electrode of silicon substrate back spatter deposition 100nm, above-mentioned both sides Au electrode all is the circle of diameter 10mm.
The surface topography of the ZnO film of processing without surface-texturing as shown in Figure 2, end grain is hexagon; The surface topography of the ZnO film of processing through surface-texturing as shown in Figure 3, surface roughness increases, and presents the pattern that height rises and falls.
With the positive pole of the connection of the front surface A u electrode in above-mentioned two kinds of devices DC power supply, the Au electrode at the silicon substrate back side connects negative pole, tests the electroluminescent spectrum of two devices under different Injection Currents.Such as Fig. 4, shown in Figure 5.Sharp peak in the spectrum is that the Random Laser by ZnO causes.Electric pumping random laser for the ZnO film after processing through surface-texturing, when Injection Current reaches only for 8mA, (as shown in Figure 4) can occur in Random Laser, and for the electric pumping random laser of the ZnO film processed without surface-texturing, when Injection Current need reach 20mA, (as shown in Figure 5) could occur in Random Laser.
Fig. 6 is the Output optical power curves of two kinds of electric pumping random lasers under different electric currents, can see: when Injection Current during greater than a certain threshold value, power output gets faster with current increases, and this is the characteristic feature of laser.Can also see in addition: the threshold current of the electric pumping random laser of the ZnO film after surface-texturing is processed is about 6mA, and the threshold current of the electric pumping random laser of the ZnO film of processing without surface-texturing is 16mA.This result illustrates that effectively ZnO film is carried out surface-texturing processes the threshold current that can reduce significantly electric pumping random laser.
Embodiment 2
1) getting resistivity is that 0.005 ohmcm, size are 15 * 15mm 2, thickness is 675 microns N-type<100〉silicon chip, puts into the reative cell of dc reactive sputtering device after the cleaning, and the reative cell vacuum is evacuated to 5 * 10 -3Pa; Utilize the method for dc reactive sputtering to deposit the thick ZnO film of about 160nm at silicon chip, when sputter, adopt simple metal Zn target, 300 ℃ of underlayer temperatures, sputtering power 100W, pass to O 2With Ar mist, O 2With the flow-rate ratio of Ar be 1: 2, operating pressure is 8Pa; Under oxygen atmosphere, 700 ℃ temperature, heat-treated 2 hours;
2) adopting concentration is the dilute hydrochloric acid solution of 0.01mol/L, to ZnO film corrosion 10 seconds, next with deionized water residual HCl solution is rinsed well under 40 ℃;
3) utilize the ZnO film of sol-gel process after processing through surface-texturing to deposit SiO 2Film, concrete steps are as follows: configuration tetraethoxysilane (TEOS): the precursor solution of ethanol (EtOH)=1: 10 (mol ratio), and the HCl that adds trace stirs after 2 hours, as SiO as catalyst 2Precursor sol.At the speed spin coating one deck SiO of above-mentioned two kinds of ZnO films with 3000 revolutions per seconds 2The precursor sol film, then 100 ℃ of lower oven dry 20 minutes, in air, formed SiO in 1 hour in 550 ℃ of heat treatments at last 2Film;
4) at SiO 2The thick translucent Au electrode of the about 20nm of sputter on the film, at the thick Au electrode of silicon substrate back spatter deposition 100nm, above-mentioned both sides Au electrode all is the circle of diameter 10mm.
ZnO film behind the above-mentioned surface-texturing of scanning electron microscopic observation shows that surface-texturing increases Film roughness, has occurred some ditch shape depressions near crystal boundary.
The positive pole that front surface A u electrode in the above-mentioned device is connected DC power supply, the Au electrode at the silicon substrate back side connects negative pole, the electroluminescent spectrum of test component under different Injection Currents, in the embodiment 1 without the ZnO film device of surface-texturing as the reference device.As shown in Figure 8, when Injection Current only was 9mA, Random Laser can occur.And for the electric pumping random laser without the ZnO film of surface-texturing, when Injection Current need reach 20mA, (as shown in Figure 5) could occur in Random Laser.The result shows, ZnO film is carried out the threshold current that surface-texturing can reduce electric pumping random laser, when the texturing condition changed, the degree that the threshold current of electric pumping random laser reduces can change thereupon.

Claims (2)

1. the preparation method of an electric pumping random laser comprises:
At substrate face deposition ZnO film, be placed on heat treated under the oxygen atmosphere, treatment temperature is 600 ~ 800 ℃, the time is 1 ~ 3 hour; Then be placed in the hydrochloric acid and corrode, the concentration of described hydrochloric acid is 0.005 ~ 0.03mol/L, and corrosion temperature is 20 ~ 50 ℃, and the time is 3 ~ 15 seconds; Taking-up cleans up, and deposits SiO at ZnO film 2Film is at substrate back and SiO 2Thin film deposition Au electrode.
2. the electric pumping random laser that makes of the described preparation method of claim 1.
CN 201110172770 2011-06-24 2011-06-24 Surface-textured-zinc oxide (ZnO)-film-based electrically pumped random laser and preparation method Expired - Fee Related CN102263373B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101510664A (en) * 2009-03-23 2009-08-19 浙江大学 Electric pumping silicon base MgxZn1-xO film ultraviolet accidental laser and preparation method thereof
CN101588021A (en) * 2009-06-10 2009-11-25 浙江大学 Electric pumping random laser of silicon zinc oxide nano-rod array

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101510664A (en) * 2009-03-23 2009-08-19 浙江大学 Electric pumping silicon base MgxZn1-xO film ultraviolet accidental laser and preparation method thereof
CN101588021A (en) * 2009-06-10 2009-11-25 浙江大学 Electric pumping random laser of silicon zinc oxide nano-rod array

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