WO2019037206A1 - 一种零功率消耗的真空紫外光伏探测器 - Google Patents

一种零功率消耗的真空紫外光伏探测器 Download PDF

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WO2019037206A1
WO2019037206A1 PCT/CN2017/105401 CN2017105401W WO2019037206A1 WO 2019037206 A1 WO2019037206 A1 WO 2019037206A1 CN 2017105401 W CN2017105401 W CN 2017105401W WO 2019037206 A1 WO2019037206 A1 WO 2019037206A1
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aln
gan
graphene
vuv
vacuum ultraviolet
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郑伟
黄丰
林日成
张召君
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Sun Yat Sen University
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    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F10/00—Individual photovoltaic cells, e.g. solar cells
    • H10F10/10—Individual photovoltaic cells, e.g. solar cells having potential barriers
    • H10F10/16—Photovoltaic cells having only PN heterojunction potential barriers
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F30/00—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors
    • H10F30/20—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors
    • H10F30/21—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation
    • H10F30/22—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation the devices having only one potential barrier, e.g. photodiodes
    • H10F30/222—Individual radiation-sensitive semiconductor devices in which radiation controls the flow of current through the devices, e.g. photodetectors the devices having potential barriers, e.g. phototransistors the devices being sensitive to infrared, visible or ultraviolet radiation the devices having only one potential barrier, e.g. photodiodes the potential barrier being a PN heterojunction

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  • the invention belongs to the field of vacuum ultraviolet light (VUV) detection technology. More specifically, it relates to the use of graphene in vacuum ultraviolet photovoltaic detectors and a zero-power consumption vacuum ultraviolet photovoltaic detector.
  • VUV vacuum ultraviolet light
  • VUV (10-200nm) detection technology is mainly used in the field of cosmic chemistry and space science, for example, to study the elemental composition and expansion of the nebula, to monitor the formation and evolution of solar storms [DNBaker et al. Science 2002., DNBaker et al. Nature 2004., MA Guerrero et al. Astronomy & Astrophysics 2013.].
  • satellite or space probes mainly use a combination system of violet spectrometers and microchannel plates for VUV detection [O. Venot et al. Astronomy & Astrophysics 2013., H. W. Moos et al. The Astrophysical Journal 2000.].
  • the semiconductor-based VUV detectors currently reported are all photoconductive detectors, which have a large gap between the sensitivity and the response speed.
  • researchers are more eager to implement a photovoltaic VUV detector than a photoconductive VUV detector because it can achieve zero power consumption and produce a charge signal proportional to the light intensity.
  • the preparation of AlN-based photovoltaic detectors faces a key technical bottleneck, and it is impossible to obtain a transparent electrode having a transmission characteristic to VUV.
  • the technical problem to be solved by the present invention is to overcome the defects and shortcomings of the above-mentioned conventional photovoltaic type VUV semiconductor-based detectors, and to meet the urgent need for a photovoltaic-type VUV detector for zero power consumption in the current space exploration, the present invention is disclosed for the first time in Application in vacuum ultraviolet photovoltaic detectors.
  • the results of the present invention have unexpectedly found that graphene (Gr) has a transmittance to VUV of more than 90%.
  • p-type Graphene is used as a transparent electrode to collect holes
  • AlN is used as a light-absorbing layer to generate photo-generated carriers.
  • the flux is constructed as a heterojunction device with PN characteristics.
  • the device The realization of the long-awaited zero-power consumption VUV photovoltaic detector is realized.
  • the device also exhibits excellent VUV response characteristics and has a good application prospect.
  • Another object of the present invention is to provide a back-to-back photovoltaic detector of p-Gr/AlN/p-GaN.
  • the invention discloses for the first time the application of graphene in the preparation of vacuum ultraviolet photovoltaic detectors.
  • the vacuum ultraviolet photovoltaic detector is a vacuum ultraviolet photodetector with zero power consumption.
  • the above application refers to the use of graphene as a VUV window for a vacuum ultraviolet photodetector.
  • the present invention also provides, for the first time, a back-to-back photovoltaic detector of p-Gr/AlN/p-GaN, a back-to-back heterojunction device of p-Gr/AlN/p-GaN, which uses graphene.
  • a back-to-back photovoltaic detector of p-Gr/AlN/p-GaN a back-to-back heterojunction device of p-Gr/AlN/p-GaN, which uses graphene.
  • As a VUV window As a VUV window.
  • the back-to-back photovoltaic detector of the p-Gr/AlN/p-GaN has AlN as a light absorbing layer.
  • the back-to-back photovoltaic detector of the p-Gr/AlN/p-GaN is constructed by the following method:
  • epitaxial AlN thin film layer firstly, a GaN buffer layer is grown on a c-plane sapphire planar substrate, then undoped GaN is grown, and regrown p-GaN is grown; then, after annealing, secondary epitaxial AlN is obtained to obtain epitaxial AlN.
  • Film layer firstly, a GaN buffer layer is grown on a c-plane sapphire planar substrate, then undoped GaN is grown, and regrown p-GaN is grown; then, after annealing, secondary epitaxial AlN is obtained to obtain epitaxial AlN.
  • the carrier concentration in the step S13 is 3 ⁇ 10 17 /cm 3 and the mobility is 10 cm 3 /V ⁇ s.
  • step S1 in the method for constructing the back-to-back photodetector device of the p-Gr/AlN/p-GaN, the specific method of step S1 is as follows:
  • step S11 is to grow a 25 nm GaN buffer layer on a c-plane sapphire planar substrate at 530 °C.
  • step S12 is to grow 2.5 ⁇ m of undoped GaN at a pressure of 200 torr at 1050 °C.
  • step S13 is to grow 200 nm p-GaN at 950 °C.
  • step S14 is annealed at 725 ° C for 10 min in a nitrogen atmosphere; last 50 torr pressure, 1050 ° C
  • the epitaxial AlN thin film layer was obtained by epitaxially epitaxially 100 nm AlN.
  • step S2 is as follows:
  • a gold wire having a diameter of 20 to 30 ⁇ m is connected to the gold electrode using a liquid Ga droplet, and an ohmic contact is directly formed on the p-GaN end using the thermally melted In as an electrode.
  • the size of the graphene transparent conductive window constructed in step S21 is 3 x 5 mm.
  • the deposition thickness of Ti in step S22 is 20 nm, and the deposition thickness of Au is 50 nm.
  • the diameter of the gold wire in step S23 is 25 ⁇ m.
  • the method for constructing the back-to-back photovoltaic detector of the p-Gr/AlN/p-GaN of the present invention is as follows:
  • a 25 ⁇ m-diameter gold wire was connected to the gold electrode using liquid Ga droplets, and an ohmic contact was constructed directly on the p-GaN end using the thermally melted In as an electrode.
  • the present invention reveals that Graphene's high (96%) light transmission characteristics in the VUV band can break through the primary key bottleneck of VUV photovoltaic devices. Further, the present invention assembles a p-type doped Graphene (without affecting VUV transmission characteristics) on a high crystalline quality AlN material to construct a heterojunction photovoltaic device having PN characteristics. The device exhibits ultra-high performance VUV spectral selection response characteristics. The device forms an open circuit voltage of 1.8V under VUV light. At 0V bias, the external quantum efficiency of the photocurrent generated by the device is as high as 42.6%, which is a thin film photoconductive type. 13.7 times the device. The response time is 80 ns under nanosecond VUV light pulse irradiation. This result is 10,000 to 1,000,000 times faster than the response of the currently reported photoconductive VUV detector.
  • the VUV photovoltaic detector is a high performance, zero power, integrated VUV photovoltaic detector.
  • the present invention finds for the first time that the transmittance of graphene to VUV is greater than 90%, and discloses for the first time the application in vacuum ultraviolet photovoltaic detectors, that is, the present invention collects holes by using p-type Graphene as a transparent electrode, and AlN as a light absorbing layer.
  • the generation of photo-generated carriers and the construction of a heterojunction device with PN characteristics provide the basis for the first development of a high-performance, zero-power, integrated VUV photodetector.
  • the VUV photovoltaic detector device of the present invention is the first to realize a long-awaited zero-power consumption semiconductor-based VUV photovoltaic detector for cosmologists and device experts.
  • the device also exhibits excellent VUV spectrally selective response characteristics, such as 13.7 times higher than the conventional device, and thanks to Gr's room temperature high mobility and high hole collection efficiency, the device A super fast time of 80 ns (10 4 to 10 6 times faster than the currently reported photoconductive VUV device) response characteristics and high EQE are achieved.
  • Figure 1 shows the transmittance of graphene to the electromagnetic wave from the VUV to the near-infrared band; the absorption near 270 nm is from the saddle point exciton.
  • FIG. 2 is a structural and electrical characteristics of the device; a cross-sectional view of the structure of the ap-Gr/AlN/p-GaN heterojunction device, b. an optical photograph of the device, a schematic diagram of the p-doping process of the c.Gr electrode, and d.
  • the IV output characteristics in the dark state in which the illustration shows the equivalent circuit of the device under different bias voltages; here, for the sake of simplicity, the internal resistance and junction capacitance of the device are ignored in the equivalent circuit.
  • Figure 3 shows the voltage noise density of the device.
  • AlN is about 100 nm
  • p-GaN is 300 nm
  • undoped GaN is 500 nm.
  • Figure 5 shows the XRD pattern of the device.
  • the (002) peaks of AlN and GaN are clearly visible, 300 and 200 arc seconds, respectively.
  • Figure 6 shows the Raman scattering of the device. The characteristic signals of the AlN, GaN and Gr components of the device are observed.
  • Fig. 7 is a photoluminescence spectrum of an AlN film having an emission center position at 214 nm.
  • Figure 8 is an ohmic contact between the p-Gr and the Ti/Au electrode.
  • Figure 9 is an ohmic contact between p-GaN and an In electrode.
  • Figure 10 is a VUV photovoltaic test and mechanism; A. Photovoltaic response of the device under 185 nm monochromatic illumination, B. Voltage output characteristics of the device under different illumination conditions, C. Device produces photovoltaic effect under VUV illumination Mechanisms.
  • Figure 11 is a time-dependent photovoltaic response test; a. Photoresponse test of the device under VUV nanosecond pulse, where the device is connected in parallel with the resistor (0.1 M ⁇ ) and the oscilloscope; b. The device is in 9 consecutive equally spaced pulses The resulting voltage output signal; c and d are respectively a magnified view and a re-magnified view of b.
  • Figure 12 is a VUV spectral response test; a. A schematic of the device for spectral response testing, b. Optical responsiveness of the device to different wavelengths of light; and an illustration depicting the equivalent circuit of the device under different illumination conditions.
  • photovoltaic detectors typically have a vertical structure of the "sandwich" type such that the photosensitive layer is in the middle of the upper and lower conductive layers, wherein the upper conductive layer must also be transparent to the probe light. Therefore, the present invention must also have a VUV transparent conductive material as a window layer of the outer layer covering the photosensitive layer to collect photogenerated carriers for the vertical structure of the VUV photovoltaic detector to be explored.
  • VUV spectral transmission experimental results are shown in Figure 1.
  • the VUV to near-infrared transmission spectrum tested in Figure 1 is by means of deep-UV spectrophotometer of Shimadzu UV- 2600, implemented).
  • Epitaxial growth of GaN and AlN was performed using 48-piece MOCVD, HICRO-I, MTM Semiconductor Equipment Co., Ltd.
  • a 25 nm GaN buffer layer was grown on a c-plane sapphire planar substrate at 530 ° C; then 2.5 ⁇ m of undoped GaN was grown at 200 torr pressure, 1050 ° C; then 200 nm was grown at 950 ° C.
  • GaN carrier concentration: 3 ⁇ 10 17 /cm 3 , mobility: 10 cm 3 /V ⁇ s); then annealed at 725 ° C for 10 min in a nitrogen atmosphere; finally 50 torr pressure, secondary epitaxial 100 nm AlN at 1050 ° C, An epitaxial AlN thin film layer was obtained.
  • Example 2 by means of the high light transmission characteristics of Gr to VUV light, we constructed a back-to-back heterojunction device of p-Gr/AlN/p-GaN as shown in Fig. 2 a and b.
  • Figure 2 shows the structure and electrical characteristics of the device; where a is a cross-sectional view of the p-Gr/AlN/p-GaN heterojunction device structure, b is an optical photo of the device, and c is a p-doping of the Gr electrode.
  • d is the IV output characteristic of the device in the dark state, and the illustration shows the equivalent circuit of the device under different bias voltages; here, for the sake of simplicity, the internal resistance and junction of the device are neglected in the equivalent circuit. capacitance.
  • Figure 4 shows the SEM image of the cross-sectional structure of the device (SEM emission is performed by the field emission scanning electron microscope of ZEISS AURIGA).
  • Figure 5 shows the XRD pattern of the device (the XRD test uses the Bruker D8 Advance X-ray diffractometer).
  • Fig. 6 shows the Raman data of the device (Rmana spectrum using Renishaw in Via reflex microRaman spectroscopy, with 514 nm pump laser), both indicating that the material of the device is constructed with high crystal quality.
  • the light absorbing layer AlN has a very symmetrical band edge emission at 215 nm (see Fig. 7), which also implies that the device has selective absorption characteristics for VUV light.
  • Figure 7 shows the photoluminescence spectrum of an AlN film with a center of luminescence at 214 nm.
  • the VUV Photoluminescence is measured using an ArF excimer laser, EX5/250 Mini Excimer Laser (GAM LASER), and the spectrum acquisition using QE65PRO Scientific- Grade Spectrometer with H70 grating (200-289 nm).
  • the IV output characteristics of the device in the dark state are consistent with the back-to-back device structure we designed. There are two distinct junction regions, a p-Gr/AlN junction with a low reverse breakdown voltage. a higher reverse breakdown voltage AlN/p-GaN junction.
  • the IV curve can be divided into three characteristic parts according to different linear relationships: I, p-Gr/AlN is forward biased, while AlN/p-GaN is reverse biased, and the device exhibits current cutoff; II, AlN/p -GaN is forward biased, while p-Gr/AlN is reverse biased, the device also exhibits current cutoff; III, AlN/p-GaN forward bias, p-Gr/AlN breakdown, device exhibits current conduction through.
  • the electrode contact (Au/Ti/p-Gr, In/p-GaN) is an ohmic contact (see Figures 8 and 9) and does not change the output characteristics of the device (voltage noise density test uses dynamic signal Analyzer of Stanford SR785).
  • the 185 nm monochromatic light source is a characteristic line from a quartz glass packaged low-pressure mercury lamp that is split by a prism; the 250 nm monochromatic light source is from a deep-UV LED.
  • the device emits a 1.8V electromotive force difference (open circuit voltage) between the two ends of the device under 185 nm monochromatic illumination (from the characteristic line of a low-pressure mercury lamp).
  • the electromotive force at the p-Gr end is higher than the electromotive force at the p-GaN end.
  • the device does not have any open circuit voltage output as in the dark state. This result, on the one hand, indicates that the device has obvious VUV spectral selection response characteristics, and on the other hand, it also indirectly confirms that the AlN absorption layer in the device has high crystalline quality and exhibits a high resistance state. This layer of AlN neither absorbs photons with energy below the bandgap to generate photogenerated carriers, nor does it allow the carriers to diffuse outward, even if additional photogenerated carriers are formed in aN.
  • the invention responds to the device with a 193 nm ns pulse laser
  • the test is shown in Figure 11 in Figure a.
  • the 193nm pulse source used for the time response test is the ArF excimer laser, INC EX5/250 Mini Excimer Laser (GAM LASER); the high-speed voltage signal acquisition device used is the 6G oscilloscope Oscilloscope KEYSIGHT DSOS604A.
  • Figure b in Figure 11 shows the results of the time-dependent photovoltaic response of the device under illumination of nine VUV plus, perfectly reproducing the optical pulse signal.
  • Table 1 compares with the reported parameters of semiconductor-based VUV detectors
  • Control 1 refers to BenMoussa, A. et al. Characterization of AlN metal-semiconductor-metal diodes in the spectral range of 44-360 nm: Photoemission assessments. Appl. Phys. Lett. 92, 022108 (2008). Balducci, A. et al. Extreme ultraviolet single-crystal diamond detectors by chemical vapor deposition. Appl. Phys. Lett. 86, 193509 (2005).
  • the device is a qualified VUV detector, and an important device parameter needs to be evaluated, that is, whether the device has VUV spectral selection response characteristics.
  • R ⁇ I/PS
  • the test system for VUV spectral response in Figure 12 is the Shimadzu UV- used. 2600 continuous adjustable light source, where the power calibration of the light source is VXUV20A photodetector (PTO DIODE CORP), and the source meter used for current test is KEITHLEY 2636b.
  • the spectrally dependent optical responsivity is shown in Figure 12, panel b, and the device's response cutoff wavelength is around 205 nm. This value is in agreement with the spectral absorption characteristics of AlN, which is attributed to the high crystal quality of the epitaxially grown AlN absorber layer in the device.
  • the inset in Figure b of Figure 12 illustrates the VUV spectral selection response.
  • p-Gr/AlN can be equivalent to a photocell (AlN absorbs VUV photons, producing positive and negative photogenerated carriers, which are opposite to each other. The direction drifts to form photocurrent).
  • the incident light wavelength ⁇ >200nm the high-resistance state of AlN is unchanged, and the photo-generated carriers generated by p-GaN absorbing deep-VU photons cannot pass through the high-resistance AlN, and can only recombine inside GaN, so the device does not generate Photocurrent.
  • the stability of the photodetector is an important parameter that can ultimately be practically applied.

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Abstract

一种石墨烯(Graphene)在真空紫外光伏探测器中的应用以及一种零功率消耗的真空紫外光伏探测器。石墨烯对真空紫外光的透过率大于90％，该真空紫外光伏探测器在高结晶质量的AlN材料上组装上p-type掺杂的石墨烯(Graphene)作为透明电极收集空穴，AlN作为吸光层产生光生载流子，构建了一个具有PN特性的异质结光伏器件。该器件实现了零功率消耗真空紫外光伏探测器的制备，该器件还表现出优秀的真空紫外响应特性，光电转换外量子效率比传统器件高13.7倍，具有80ns的超快响应时间，比现有光电导型真空紫外器件快104～106倍，具有很好的应用前景。

Description

一种零功率消耗的真空紫外光伏探测器 技术领域
本发明属于真空紫外光(VUV)探测技术领域。更具体地，涉及石墨烯在真空紫外光伏探测器中的应用以及一种零功率消耗的真空紫外光伏探测器。
背景技术
VUV(10-200nm)探测技术主要应用于宇宙化学和太空科学领域，例如用于研究星云的元素组成和扩张，监测太阳风暴的形成和演变等[D.N.Baker等.Science 2002.,D.N.Baker等.Nature 2004.,M.A.Guerrero等.Astronomy&Astrophysics 2013.]。目前，卫星或宇宙探测器主要使用紫罗兰色谱仪和微通道板的组合系统来进行VUV的探测[O.Venot等.Astronomy&Astrophysics 2013.,H.W.Moos等.The Astrophysical Journal 2000.]。然而这些传统探测系统具有体积笨重、功耗高(数千伏的驱动电压)等缺点，这些缺点给卫星的运行带来的过高的供电负担，同时也提高了卫星的反射成本。材料和器件科学家们一直在努力为宇宙学家们寻找新的方案，尝试发展基于宽禁带半导体材料(例如主流的AlN)的低功耗、轻便、小型的VUV探测器[W.Zheng等.Adv.Mater.2015.,J.Li等.Appl.Phys.Lett.2006.]。
目前报道的半导体基VUV探测器，都是光电导型探测器，在灵敏度和响应速度上都离真实应用有较大差距。事实上，面对真实的应用需求，相比于光电导型VUV探测器，研究者更期望实现光伏型VUV探测器，因为它能实现零功率消耗且自己产生正比于光照强度的电荷信号。然而，当前的技术条件下，制备AlN基光伏探测器面临一个关键的技术瓶颈，无法获得对VUV具有透过特性的透明电极。
在过去二十年中，宇宙学家和材料科学家一直在研究开发具有低功耗和小尺寸的新一代基于半导体的VUV探测器，替代传统沉重且具有高能耗的微通道探测系统，以降低卫星的电力负荷和发射卫星的成本。然而，能实现零功率消耗的光伏型VUV半导体基探测器，作为一个最被希望实现的目标，始终没有得到实现。
发明内容
本发明要解决的技术问题是克服上述现有光伏型VUV半导体基探测器的缺陷和不足，以及为了满足当前宇宙探索对零功率消耗的光伏型VUV探测器的迫切需求，本发明首次公开了在真空紫外光伏探测器中的应用。本发明的研究结果出乎意料的发现，石墨烯(Graphene，Gr)对VUV的透过率大于90％，本发明将p-type的Graphene作为透明电极收集空穴，AlN作为吸光层产生光生载流子，构建了一个具有PN特性的异质结器件。该器件 实现了人们期望已久的零功率消耗VUV光伏探测器的制备，该器件还表现出优秀的VUV响应特性，具有很好的应用前景。
本发明的目的是提供石墨烯在真空紫外光伏探测器中的应用。
本发明另一目的是提供一种p-Gr/AlN/p-GaN的背靠背光伏探测器件。
本发明上述目的通过以下技术方案实现：
本发明首次公开了石墨烯在制备真空紫外光伏探测器中的应用。
具体地，所述真空紫外光伏探测器为零功率消耗的真空紫外光伏探测器。
优选地，上述应用是指石墨烯作为真空紫外光伏探测器的VUV窗口的应用。
本发明还首次提供了一种p-Gr/AlN/p-GaN的背靠背光伏探测器件，即一种p-Gr/AlN/p-GaN的背靠背异质结器件，该器件使用石墨烯(graphene)作为VUV窗口。
进一步地，所述p-Gr/AlN/p-GaN的背靠背光伏探测器件以AlN为吸光层。
优选地，所述p-Gr/AlN/p-GaN的背靠背光伏探测器件由如下方法构建得到：
S1.外延AlN薄膜层的生长：首先在c面蓝宝石平面衬底上生长GaN缓冲层，然后生长非掺杂的GaN，再生长p-GaN；然后退火处理后，二次外延AlN，得到外延AlN薄膜层；
S2.器件的制备：首先在外延AlN薄膜层表面构建石墨烯作为透明导电窗口，然后在石墨烯的一端依次沉积Ti和Au；最后使用液态Ga液滴将金线与金电极进行连接，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
其中，步骤S13的载流子浓度为3×1017/cm3,迁移率为10cm3/V·s。
另外，优选地，所述p-Gr/AlN/p-GaN的背靠背光伏探测器件的构建方法中，步骤S1的具体方法如下：
S11.在500～550℃条件下，在c面蓝宝石平面衬底上生长20～30nm GaN缓冲层；
S12.然后在180～220torr压力、1000～1100℃下生长2～3μm的非掺杂的GaN；
S13.然后再在900～1000℃下生长180～220nm p-GaN；
S14.然后在氮气气氛中700～750℃退火8～15min；最后40～60torr压力、1000～1100℃下二次外延80～120nm AlN，得到外延AlN薄膜层。
更优选地，步骤S11是在530℃条件下，在c面蓝宝石平面衬底上生长25nm GaN缓冲层。
更优选地，步骤S12是在200torr压力、1050℃下生长2.5μm的非掺杂的GaN。
更优选地，步骤S13是在950℃下生长200nm p-GaN。
更优选地，步骤S14是在氮气气氛中725℃退火10min；最后50torr压力、1050℃ 下二次外延100nm AlN，得到外延AlN薄膜层。
优选地，所述p-Gr/AlN/p-GaN的背靠背光伏探测器件的构建方法中，步骤S2的具体方法如下：
S21.利用湿法转移的方法，在外延AlN薄膜层表面构建石墨烯作为透明导电窗口；
S22.利用热蒸镀的方法在石墨烯的一端沉积15～25nm Ti，然后再沉积40～60nm Au；
S23.使用液态Ga液滴将20～30μm直径的金线与金电极进行连接，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
更优选地，步骤S21中构建的石墨烯透明导电窗口的尺寸为3×5mm。
更优选地，步骤S22中Ti的沉积厚度为20nm，Au的沉积厚度为50nm。
更优选地，步骤S23中所述金线的直径为25μm。
综上所述，最优选地，本发明所述p-Gr/AlN/p-GaN的背靠背光伏探测器件的构建方法如下：
S1.外延AlN薄膜层的生长
S11.在530℃条件下，在c面蓝宝石平面衬底上生长25nm GaN缓冲层；
S12.然后在200torr压力、1050℃下生长2.5μm的非掺杂的GaN；
S13.然后再在950℃下生长200nm p-GaN(载流子浓度为3×1017/cm3,迁移率为10cm3/V·s)；
S14.然后在氮气气氛中725℃退火10min；最后50torr压力、1050℃下二次外延100nm AlN，得到外延AlN薄膜层；
S2.器件的制备
S21.利用湿法转移的方法，在外延AlN薄膜层表面构建3×5mm的石墨烯作为透明导电窗口；
S22.利用热蒸镀的方法在石墨烯的一端沉积20nm Ti，然后再沉积50nm Au；
S23.使用液态Ga液滴将25μm直径的金线与金电极进行连接，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
本发明首次在实验上揭示了Graphene在VUV波段高(96％)透光特性，可突破VUV光伏器件的首要关键瓶颈。进一步，本发明在高结晶质量的AlN材料上组装上了p-type掺杂的Graphene(并不影响VUV透过特性)，构建一个具有PN特性的异质结光伏器件。该器件展现出超高性能的VUV光谱选择响应特性。在VUV光辐照下，该器件形成一个1.8V的开路电压。在0V偏压下，器件产生光电流的外量子效率高达42.6％，是薄膜光电导型 器件的13.7倍。在纳秒VUV光脉冲辐照下，其响应时间为80ns。这一结果比当前报道的光电导型VUV探测器的响应速度快10,000到1,000,000倍。
因此，本发明所构建的p-Gr/AlN/p-GaN的背靠背光伏探测器件在制备零功耗VUV光伏探测器方面的应用，以及由此构建的零功耗VUV光伏探测器，也都应在本发明的保护范围之内。所述VUV光伏探测器为高性能、零功耗、可集成的VUV光伏探测器。
发明具有以下有益效果：
本发明首次发现石墨烯对VUV的透过率大于90％，并首次公开了在真空紫外光伏探测器中的应用，即本发明将p-type的Graphene作为透明电极收集空穴，AlN作为吸光层产生光生载流子，构建了一个具有PN特性的异质结器件，为高性能、零功耗、可集成的VUV光伏探测器的首次开发提供了基础。
本发明的VUV光伏探测器件首次实现了宇宙学家和器件专家们期待已久的零功率消耗的半导体基VUV光伏探测器。该器件还表现出优秀的VUV光谱选择性响应特性，例如：比传统器件高13.7倍的光电转换外量子效率，此外，得益于Gr的室温高迁移率和高的空穴收集效率，该器件实现了80ns的超快时间(比当前报道的光电导型VUV器件快104～106倍)响应特性和高的EQE。
附图说明
图1为石墨烯对VUV到near-infrared波段电磁波的透过率；其中270nm附近的吸收是来自于鞍点激子吸。
图2为器件的结构和电学特性；a.p-Gr/AlN/p-GaN异质结器件结构的截面图，b.器件的光学照片，c.Gr电极进行p-doping过程的示意图，d.器件在暗态下的I-V输出特性，其中插图给出了器件在不同偏压下的等效电路；这里为了表达简洁，等效电路中忽略了器件的内阻和结电容。
图3为器件的电压噪声密度。
图4为器件截面结构的SEM照片，其中AlN约为100nm,p-GaN为300nm,非掺杂GaN为500nm。
图5为器件的XRD图谱，AlN和GaN的(002)峰清晰可见，分别为300和200弧秒。
图6为器件的Raman散射图谱，器件组成部分的AlN，GaN和Gr的特征信号都观测到。
图7为AlN薄膜的光致发光光谱，其发光中心位置在214nm。
图8为p-Gr与Ti/Au电极之间的欧姆接触。
图9为p-GaN与In电极之间的欧姆接触。
图10为VUV光伏测试和机制；A.器件在185nm单色光的辐照下的光伏响应测示意图，B.器件在不同光照状态下的电压输出特性，C.器件在VUV光照下产生光伏效应的机制。
图11为时间依赖的光伏响应测试；a.在VUV纳秒脉冲下器件的光响应测试示意图,其中器件与电阻(0.1 MΩ)和示波器之间相互并联；b.器件在9个连续等间隔脉冲下产生的电压输出信号；c和d分别是b中局部的放大图和再放大图。
图12为VUV光谱响应测试；a.器件进行光谱响应测试的示意图，b.器件对不同光波长的光学响应度；其中插图描述了器件在不同光照下的器件等效电路。
具体实施方式
以下结合说明书附图和具体实施例来进一步说明本发明，但实施例并不对本发明做任何形式的限定。除非特别说明，本发明采用的试剂、方法和设备为本技术领域常规试剂、方法和设备。
除非特别说明，以下实施例所用试剂和材料均为市购。
实施例1石墨烯对VUV光透明的研究
众所周知，通常光伏探测器必须具有类“三明治”型的垂直结构，使其光敏层处于上下导电层中间，其中上导电层还必须对探测光透明。因此，本发明对于要探索的垂直结构的VUV光伏探测器，也必须要具有VUV透明导电材料作为外层的窗口层覆盖光敏层来收集光生载流子。
我们经过大量的探索研究发现，石墨烯对VUV具有高的透过率，VUV光谱透射实验结果见图1(图1中测试的VUV到near-infrared透射光谱是借助deep-UV spectrophotometer of Shimadzu UV-2600，实现的)。
典型的，在185-200nm VUV波段内，石墨烯的透过率依然高达96％，几乎和可见光的透过率一样高。这一结果，为实现VUV光伏器件提供了理论可行的依据。
实施例2 VUV光伏器件的制备
1、薄膜(Thin films)外延生长：
外延生长GaN和AlN使用的是48片生产型MOCVD,HICRO-I，MTM Semiconductor Equipment Co.,Ltd。
首先，在530℃条件下，在c面蓝宝石平面衬底上生长25nm GaN缓冲层；然后在 200torr压力、1050℃下生长2.5μm的非掺杂的GaN；然后再在950℃下生长200nm p-GaN(载流子浓度为3×1017/cm3,迁移率为10cm3/V·s)；然后在氮气气氛中725℃下退火10min；最后50torr压力、1050℃下二次外延100nm AlN，得到外延AlN薄膜层。
2、器件制备：
在生长了外延AlN薄膜层后，我们使用湿法转移的方法，在AlN表面构建了3×5mm的石墨烯作为透明导电窗口。随后使用热蒸镀的方法在石墨烯的一端先沉积了20nm Ti，然后再沉积了50nm Au。然后，使用液态Ga液滴将25μm直径的金线与金电极进行连接。另一方面，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
实施例3 VUV光伏器件的表征
如实施例2，借助Gr对VUV光的高透光特性，我们构建了一个如图2中a图和b图所示的p-Gr/AlN/p-GaN的背靠背异质结器件。图2为器件的结构和电学特性；其中，a图为p-Gr/AlN/p-GaN异质结器件结构的截面图，b图为器件的光学照片，c图为Gr电极进行p-doping过程的示意图，d图为器件在暗态下的I-V输出特性，其中插图给出了器件在不同偏压下的等效电路；这里为了表达简洁，等效电路中忽略了器件的内阻和结电容。
值得特别说明的是，为了能实现背靠背的光伏器件，这里我们有意借助硝酸蒸汽对Gr电极进行了p-doping(如图2中c图，H.Yan等人Nature Nanotech.2012)。这种背靠背的结构具有的明显优势是：在零偏压下，器件的中正、负载流子的热扩散都能得到抑制，因此能实现更低的电压噪声密度(见图3)，这有利于监测极其微弱的VUV光信号。
图4给出了器件截面结构的SEM照片(SEM测试使过的是field emission scanning electron microscope of ZEISS AURIGA)，图5给出了器件的XRD图谱(XRD测试使用的是Bruker D8 Advance X-ray diffractometer)，图6给出了器件的Raman数据(Rmana光谱使用的是Renishaw inVia reflex microRaman spectroscopy,with 514 nm pump laser)，都表明构建器件的材料具有高的结晶质量。另外，作为器件核心部分吸光层AlN，在215nm处有很清晰对称的带边发射(见图7)，也暗示了该器件具有对VUV光具有选择吸收的特性。图7为AlN薄膜的光致发光光谱，其发光中心位置在214nm，其中，VUVPhotoluminescence的测量使用的是ArF准分子激光器，EX5/250 Mini Excimer Laser(GAM LASER),光谱采集使用的是QE65PRO Scientific-Grade Spectrometer with H70 grating(200-289nm)。
器件在暗态下的I-V输出特性(图2中d图)，与我们设计的背靠背器件结构吻合，存在两个明显的结区，即一个反向击穿电压低的p-Gr/AlN结和一个反向击穿电压较高 的AlN/p-GaN结。I-V曲线依据不同的线性关系可以被划分为三个特征部分：I,p-Gr/AlN正向偏置，而AlN/p-GaN反向偏置，器件表现为电流截止；II,AlN/p-GaN正向偏置，而p-Gr/AlN反向偏置，器件也表现为电流截止；III,AlN/p-GaN正向偏置，p-Gr/AlN击穿，器件表现为电流导通。这里需要强调的是电极接触(Au/Ti/p-Gr,In/p-GaN)都为欧姆接触(见图8和图9)不会改变器件的输出特性(电压噪声密度测试是使用dynamic signal analyzer of Stanford SR785)。
实施例4 VUV光伏器件的光电测试(光伏响应和机制)
进一步，我们对该器件进行了一系列的VUV光探测的测试。如图10的光伏效应测试，185nm单色光源是来自于石英玻璃封装的低压汞灯通过棱镜分光后的特征谱线；250nm单色光源来自deep-UV LED。
如图10中A图所示，器件在185nm单色光照射下(来自于低压汞灯的特征谱线)，在器件的两端之间产生了1.8V的电动势差(开路电压，见图10中B图)，其中p-Gr端的电动势要高于p-GaN端的电动势。而在250nm光照下，器件没有任何开路电压的输出同暗态下的情况一样。这一结果，一方面表明器件存在明显的VUV光谱选择响应特性，另一方面也间接证实了器件中AlN吸收层具有高结晶质量且呈现高阻状态。这层AlN既不会吸收能量低于带隙的光子产生光生载流子,也不允许载流子向外扩散，即使在aN中形成的额外光生载流子。
器件在VUV光照下，产生光伏效应的机制如图10中C图所示。当VUV光穿透Gr进入AlN后，大部分会在p-Gr/AlN间形成的空间电荷区内被吸收，产生光生电子-空穴对。他们会被空间电荷区的内建电场(E)立即分离：空穴向p-Gr漂移，而电子则向反方向漂移。最终在克服器件的内阻后在器件两端形成了一个1.8V的开路电压，成为一个具有光伏响应特性的VUV探测器.
这里值得说明的是，AlN/p-GaN之间也存在一个空间电荷区，区内也包涵一个内建电场(E1)，它对光生载流子分离的作用与E in p-Gr/AlN相反。对于我们当前的情况，我们认为VUV主要在p-Gr/AlN结区内被吸收，被埋藏更深的AlN/p-GaN结进行吸收的几率很微小，因为微弱的VUV光很难穿透100nm的AlN。所以，在当前以石墨烯为VUV窗口的探测模式下，器件产生的光生电动势的主要贡献来自于p-Gr/AlN异质结。
实施例5 VUV光伏器件的的光电测试(超快时间响应)
相比与常规的光电导型探测器，光伏探测型探测器件除了零功耗的优势外，还有一个重要优势是可以实现更高的响应速度。本发明借助193nm的ns脉冲激光，对器件进行了时间响应 测试，如图11中a图所示。时间响应测试使用的193nm脉冲光源是ArF准分子激光器，INC EX5/250 Mini Excimer Laser(GAM LASER)；使用的高速电压信号采集装置是6G示波器Oscilloscope KEYSIGHT DSOS604A。
图11中b图显示了器件在9个VUV plus的光照下时间依赖的光伏响应的结果，完好地再现光脉冲信号。
为了更清晰的分析器件的速度of时间响应，我们对图11中b图中的一个典型脉冲进行了放大(图11中c图)和再放大(图11中d图)。让我们意想不到的是，器件的上升响应时间只有短短的80ns，这一结果比当前报道过的VUV探测器件快了104～106倍(见表1)，并且经过了大量实验验证。
表1与现有报道的半导体基VUV探测器的指标参数的对比
Figure PCTCN2017105401-appb-000001
注：对照1引用BenMoussa,A.et al.Characterization of AlN metal-semiconductor-metal diodes in the spectral range of 44-360 nm:Photoemission assessments.Appl.Phys.Lett.92,022108(2008).对照2引用Balducci,A.et al.Extreme ultraviolet single-crystal diamond detectors by chemical vapor deposition.Appl.Phys.Lett.86,193509(2005)。
我们分析，这个超快的上升光响应速度归因于Gr高迁移率和AlN的高结晶质量。前者决定了光生载流子(空穴)快速的收集和传输，后者减少了缺陷对载流子(主要是空穴)束缚的概率。另一方面，器件在关段时的衰减时间存在相对较长的拖尾，这一现象在脉冲响应测试内是常见的，它不仅决定于器件本身对载流子分离和收集的速度，还取决于测试电路，仪表探头内在的阻抗和电容效应。
实施例6 VUV光伏器件的光电测试(器件中的VUV光谱选择响应)
器件是否为合格VUV探测器，还有一个重要的器件参量需要进行评价，即器件是否具有VUV光谱选择响应特性。这里，我们借助于氘灯光源和单色仪组合实现的连续可调的单色光，从VUV到deep-UV光，对器件额光响应度进行了逐个波长的测试。其中光响应度是光电探测器对单色光探测能力的指标，定义为：R＝△I/PS，其中△I是光电流Ip减去暗电流Id，P为入射光功率密度，S为器件的吸光面积。
结果如图12所示。图12中进行VUV光谱响应的测试系统是使用的Shimadzu UV- 2600的连续可调光源，其中光源的功率校准使用的是VXUV20A photodetector(PTO DIODE CORP)，电流测试使用的源表SourceMeter是KEITHLEY 2636b。
光谱依赖的光响应度如图12中b图所示，器件的响应截止波长位于205nm附近。这一值与AlN的光谱吸收特性吻合，得益于器件中外延生长的AlN吸收层具有高的结晶质量。器件在195nm的外部量子效率(EQE＝hcR/eλ，其中h为普朗克常数，c为光速，e为电子电荷，λ为入射光波长)是42.6％，见表1，是传统AlN基光电导探测器外量子效率的13.7倍。
图12中b图中插图对VUV光谱选择响应做出了解释。当入射光波长λ<200nm时，如同图10中c给出的光伏机制，p-Gr/AlN可以等效为一个光电池(AlN吸收VUV光子，产生正、负光生载流子，相互沿着相反的方向漂移，形成光电流)。当入射光波长λ>200nm时，AlN的高阻状态不变，p-GaN吸收deep-VU光子产生的光生载流子无法穿越过高阻的AlN，只能在GaN内部复合，因此器件不产生光电流。
实施例7 VUV光伏器件的稳定性
光电探测器的稳定性是最终能否实际应用的一个重要参数，为了验证本发明所得器件的稳定性，我们对器件做了其光响应长时间稳定性的测试。器件在空气中存放一个月后，其光电流没有明显变化，表明器件具有高的环境稳定性。
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其他的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (10)

  1. 石墨烯在制备真空紫外光伏探测器中的应用。
  2. 根据权利要求1所述的应用，其特征在于，所述真空紫外光伏探测器为零功率消耗的真空紫外光伏探测器。
  3. 根据权利要求1所述的应用，其特征在于，石墨烯作为真空紫外光伏探测器的VUV透明导电窗口。
  4. 一种p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，使用石墨烯作为VUV透明导电窗口。
  5. 根据权利要求4所述p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，以AlN为吸光层。
  6. 根据权利要求4所述p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，由如下方法构建得到：
    S1.外延AlN薄膜层的生长：首先在c面蓝宝石平面衬底上生长GaN缓冲层然后生长非掺杂的GaN，再生长p-GaN；然后退火处理后，二次外延AlN，得到外延AlN薄膜层；
    S2.器件的制备：首先在外延AlN薄膜层表面构建石墨烯作为透明导电窗口，然后在石墨烯的一端依次沉积Ti和Au；最后使用液态Ga液滴将金线与金电极进行连接，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
  7. 根据权利要求6所述p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，步骤S1的具体方法如下：
    S11.在500～550℃条件下，在c面蓝宝石平面衬底上生长20～30nm GaN缓冲层；
    S12.然后在180～220torr压力、1000～1100℃下生长2～3μm的非掺杂的GaN；
    S13.然后再在900～1000℃下生长180～220nm p-GaN；
    S14.然后在氮气气氛中700～750℃退火8～15min；最后40～60torr压力、1000～1100℃下二次外延80～120nm AlN，得到外延AlN薄膜层。
  8. 根据权利要求7所述p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，步骤S13的载流子浓度为3×1017/cm3,迁移率为10cm3/V·s。
  9. 根据权利要求6所述p-Gr/AlN/p-GaN的背靠背光伏探测器件，其特征在于，步骤S2的具体方法如下：
    S21.利用湿法转移的方法，在外延AlN薄膜层表面构建石墨烯作为透明导电窗口；
    S22.利用热蒸镀的方法在石墨烯的一端沉积15～25nm Ti，然后再沉积40～60nm Au；
    S23.使用液态Ga液滴将20～30μm直径的金线与金电极进行连接，在p-GaN一端直接使用热熔化的In作为电极构建欧姆接触。
  10. 权利要求4～9任一所述p-Gr/AlN/p-GaN的背靠背光伏探测器件在制备零功耗VUV光伏探测器方面的应用。
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