WO2023168996A1 - Structured superconducting-tape single photon detector and preparation method therefor - Google Patents

Structured superconducting-tape single photon detector and preparation method therefor Download PDF

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WO2023168996A1
WO2023168996A1 PCT/CN2022/134848 CN2022134848W WO2023168996A1 WO 2023168996 A1 WO2023168996 A1 WO 2023168996A1 CN 2022134848 W CN2022134848 W CN 2022134848W WO 2023168996 A1 WO2023168996 A1 WO 2023168996A1
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superconducting
structured
electron beam
superconducting strip
single photon
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张蜡宝
李飞燕
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南京大学
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    • G01JMEASUREMENT OF INTENSITY, VELOCITY, SPECTRAL CONTENT, POLARISATION, PHASE OR PULSE CHARACTERISTICS OF INFRARED, VISIBLE OR ULTRAVIOLET LIGHT; COLORIMETRY; RADIATION PYROMETRY
    • G01J1/00Photometry, e.g. photographic exposure meter
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Abstract

Disclosed in the present invention is a structured superconducting-tape single photon detector. In the present invention, the photon response sensitivity of a superconducting tape is improved by means of structure regulation and control, and the requirements of a conventional superconducting single photon detector regarding the width of a superconducting tape are reduced, such that high-sensitivity single-photon detection can be realized; and the structured superconducting-tape single photon detector is characterized in having a large detection area and a high speed, being simple in terms of preparation, being easily expandable to a large-scale array structure, etc. The single photon detector sequentially comprises, from bottom to top: a substrate, a structured superconducting tape, an electrode, an optical dielectric layer and an optical reflection layer. The preparation method mainly comprises: depositing a superconducting thin film on a surface of a substrate by means of magnetron sputtering; preparing a metal electrode on the superconducting thin film by means of photolithography and stripping technology; preparing on the superconducting thin film a structured superconducting tape shape by means of electron beam lithography technology and reactive ion etching technology; and respectively depositing an optical dielectric layer and a metal reflection layer on the surface of the structured superconducting tape by means of chemical vapor deposition technology and electron beam evaporation technology, which optical dielectric layer and metal reflection layer serve as optical cavities.

Description

结构化超导带单光子探测器及其制备方法Structured superconducting strip single-photon detector and preparation method thereof 技术领域Technical field
本发明涉及光探测技术领域,具体涉及一种结构化超导带单光子探测器及其制备方法。The invention relates to the field of light detection technology, and specifically to a structured superconducting strip single photon detector and a preparation method thereof.
背景技术Background technique
超导纳米线单光子探测器(Superconducting Nanowire Single Photon Detector,SNSPD)作为光极限探测的强有力工具,经过二十多年来的快速发展,SNSPD具有高效的探测效率、超低的暗计数、超高的时间分辨率和宽的响应频谱。这些优异的性能使其在众多的单光子探测器中脱颖而出,在诸如深空光通信、量子光学、生物荧光成像、激光雷达、暗物质探测等领域具有很好的应用前景。Superconducting Nanowire Single Photon Detector (SNSPD) is a powerful tool for light limit detection. After more than 20 years of rapid development, SNSPD has high detection efficiency, ultra-low dark count, and ultra-low dark count. High temporal resolution and wide response spectrum. These excellent properties make it stand out among many single photon detectors and have good application prospects in fields such as deep space optical communications, quantum optics, biofluorescence imaging, lidar, and dark matter detection.
传统的SNSPD通常用80~100nm宽的蜿蜒纳米线结构填充在20μm×20μm面积上作为探测器的光敏面,利用单模光纤对SNSPDs进行光耦合。在实际的应用中,探测器需要更大的光敏面来有效进行自由空间耦合或多模光纤耦合(芯直径大于50μm),常规的小面积SNSPDs已无法满足应用需求。因此,制备具有大光敏面积和高性能的SNSPD成为未来一个必然的趋势。Traditional SNSPDs usually fill a 20 μm × 20 μm area with meandering nanowire structures with a width of 80 to 100 nm as the photosensitive surface of the detector, and use single-mode optical fibers to optically couple the SNSPDs. In practical applications, detectors require larger photosensitive surfaces to effectively perform free space coupling or multimode fiber coupling (core diameter greater than 50 μm), and conventional small-area SNSPDs can no longer meet application needs. Therefore, the preparation of SNSPD with large photosensitive area and high performance has become an inevitable trend in the future.
目前,提高SNSPD光敏面积的方法包括:一方面是通过增加纳米线的长度来扩展单个像元探测器的面积,但是探测器的动态电感会随着纳米线的长度的增加而增加,这样将影响器件的恢复时间和最大计数率。另一方面是采用阵列SNSPD来提高探测器的面积,但随着阵列数目的增加,对SNSPD的读出电路具有巨大的挑战。这些方法中,随着SNSPD面积的扩大,在制备过程中纳米线的几何缺陷是无可避免的,这将影响探测器的均匀性和成品率,最终探测器的各方面性能被削减。如何制备大面积、高效率、高速度的阵列超导单光子探测器的同时减小相关负面影响已成为一个急需解决的问题。Currently, methods to increase the photosensitive area of SNSPD include: on the one hand, expanding the area of a single pixel detector by increasing the length of the nanowire. However, the dynamic inductance of the detector will increase as the length of the nanowire increases, which will affect The recovery time and maximum count rate of the device. On the other hand, array SNSPD is used to increase the area of the detector. However, as the number of arrays increases, it poses a huge challenge to the SNSPD readout circuit. In these methods, as the SNSPD area expands, geometric defects of the nanowires during the preparation process are inevitable, which will affect the uniformity and yield of the detector, and ultimately all aspects of the detector's performance will be reduced. How to prepare large-area, high-efficiency, high-speed array superconducting single-photon detectors while reducing related negative effects has become an urgent problem to be solved.
发明内容Contents of the invention
发明目的:为了制备大面积超导单光子探测器,以及为了提高在制备过程中探测器的均匀性和成品率,本发明提出了一种结构化超导带单光子探测器及其制备方法。Purpose of the invention: In order to prepare a large-area superconducting single-photon detector and to improve the uniformity and yield of the detector during the preparation process, the present invention proposes a structured superconducting strip single-photon detector and a preparation method thereof.
技术方案:结构化超导带单光子探测器,从下至上依次包括:衬底、位于衬底表面的结构化超导带、位于所述结构化超导带的尾端连接处的电极、位于所述结构化超导带表面的光学介质层和位于所述光学介质层表面的光学反射层;其中,所述结构化超导带是在超导带上设计具有微纳结构的图形,所述具有微纳结构的图形包括多个微纳孔结构,所述微纳孔结构为封闭形孔洞结构,所述封闭形孔洞结构包括但不限于圆孔、椭圆孔、方孔、矩形孔和和机翼孔。Technical solution: a structured superconducting strip single photon detector, including from bottom to top: a substrate, a structured superconducting strip located on the surface of the substrate, an electrode located at the tail end connection of the structured superconducting strip, The optical medium layer on the surface of the structured superconducting tape and the optical reflective layer on the surface of the optical medium layer; wherein the structured superconducting tape is designed with a micro-nano structure pattern on the superconducting tape, and the Patterns with micro-nano structures include multiple micro-nano pore structures, and the micro-nano pore structures are closed hole structures. The closed hole structures include but are not limited to round holes, elliptical holes, square holes, rectangular holes, and machine holes. Wing holes.
所述结构化超导带由超导薄膜组成,其结构为首尾相连的蜿蜒结构。The structured superconducting strip is composed of a superconducting film, and its structure is a meandering structure connected end to end.
所述结构化超导带的宽度在0.1~20μm,超导带的填充率为0.1~0.9。The width of the structured superconducting strip is 0.1-20 μm, and the filling rate of the superconducting strip is 0.1-0.9.
所述微纳结构的特征为沿着超导带方向的横向宽度为超导带宽度的3%~95%。The characteristic of the micro-nano structure is that the lateral width along the direction of the superconducting strip is 3% to 95% of the width of the superconducting strip.
在本发明中,通过将结构化超导带设计为首尾相连的蜿蜒形状来提高探测器的填充率,结构化超导带是在超导带上设计具有一定尺寸微纳孔阵列结构来调控超导带的磁通的产生和穿越,有助于探测器对单光子的响应。光学介质层和光学反射层的存在可以提高结构化超导带对单光子的吸收率,从而提高结构化超导带单光子探测器的探测效率。由于结构化超导带的宽度是微米量级的,相比于传统的纳米线,制备具有良好均匀性的大面积的结构化超导带单光子探测器更加容易。In the present invention, the filling rate of the detector is improved by designing the structured superconducting strip into a meandering shape connected end to end. The structured superconducting strip is controlled by designing a micro-nanohole array structure with a certain size on the superconducting strip. The generation and passage of magnetic flux in the superconducting ribbon contributes to the detector's response to single photons. The existence of the optical medium layer and the optical reflection layer can increase the absorption rate of single photons by the structured superconducting strip, thereby improving the detection efficiency of the structured superconducting strip single photon detector. Since the width of structured superconducting strips is on the order of micrometers, it is easier to prepare large-area structured superconducting strip single-photon detectors with good uniformity than traditional nanowires.
本发明还公开了一种结构化超导带单光子探测器的制备方法,包括以下步骤:The invention also discloses a method for preparing a structured superconducting strip single photon detector, which includes the following steps:
步骤1:采用磁控溅射技术,在衬底上生长一层超导薄膜;Step 1: Use magnetron sputtering technology to grow a layer of superconducting film on the substrate;
步骤2:在超导薄膜上生长电极;Step 2: Grow electrodes on the superconducting film;
步骤3:采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到具有微纳结构的超导带形状。Step 3: Use electron beam exposure technology and reactive ion etching technology to transfer the micro-nano structure pattern to the superconducting film to obtain the superconducting strip shape with micro-nano structure.
步骤4:根据步骤3,其特征在于,在所述采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到结构化超导带形状之后,还包括以下步骤:Step 4: According to step 3, it is characterized in that, after using electron beam exposure technology and reactive ion etching technology to transfer the pattern of the micro-nanopore structure to the superconducting film to obtain the structured superconducting strip shape, it also includes Following steps:
采用化学气相沉积法在具有微纳结构的超导带的表面上沉积一层二氧化硅作为光学介质层;A chemical vapor deposition method is used to deposit a layer of silicon dioxide as an optical medium layer on the surface of a superconducting strip with a micro-nano structure;
采用电子束蒸发和剥离技术在光学介质层的表面上生长一层金作为光学反射层。Electron beam evaporation and lift-off techniques are used to grow a layer of gold on the surface of the optical medium layer as an optical reflective layer.
步骤5:根据步骤3,其特征在于,所述采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到结构化超导带形状具体包括:Step 5: According to step 3, it is characterized in that the use of electron beam exposure technology and reactive ion etching technology to transfer the pattern of the micro-nanopore structure to the superconducting film to obtain the shape of the structured superconducting strip specifically includes:
在具有电极的超导薄膜上旋涂正性电子束抗刻蚀胶作为电子束抗刻蚀层;Spin-coating the positive electron beam etching resist on the superconducting film with the electrode as the electron beam etching resisting layer;
采用电子束曝光技术在具有电子束抗刻蚀层的薄膜上根据微纳结构的图形进行曝光,采用显影和定影处理在电子束抗刻蚀层上得到微纳结构的图形;Electron beam exposure technology is used to expose the film with an electron beam etching-resistant layer according to the pattern of the micro-nano structure, and development and fixing processes are used to obtain the pattern of the micro-nano structure on the electron beam etching-resistant layer;
采用反应离子刻蚀技术将微纳孔结构的图形转移至薄膜上,得到具有结构化超导带形状;Reactive ion etching technology is used to transfer the pattern of micro-nanopore structure to the film to obtain a structured superconducting strip shape;
利用N-甲基吡咯烷酮溶液水浴超声去除结构化超导带表面残留的正性电子束抗刻蚀胶,最终得到表面干净的结构化超导带。N-methylpyrrolidone solution water bath ultrasonic was used to remove the positive electron beam etching resist remaining on the surface of the structured superconducting tape, and finally a structured superconducting tape with a clean surface was obtained.
步骤6:根据步骤5,其特征在于:在电子束曝光技术中,采用2nA的电子束流在具有电子束抗刻蚀层的薄膜上绘制微纳结构的图形,曝光剂量为600μC/cm 2Step 6: According to step 5, it is characterized in that: in the electron beam exposure technology, an electron beam current of 2nA is used to draw the pattern of the micro-nano structure on the film with an electron beam etching resistant layer, and the exposure dose is 600 μC/cm 2 .
有益效果:本发明与现有技术相比,具有以下优点:Beneficial effects: Compared with the existing technology, the present invention has the following advantages:
(1)本发明提供了一种结构化超导带的思路来制备大面积的超导带单光子探测器, 通过结构调控增加超导带对光子响应灵敏度,降低了常规超导单光子探测器对超导带宽度的要求,微米宽的结构化超导带允许大光敏面积探测器的制备,在实现单光子探测的同时,降低工艺制备难度,具有制备难度低以及耦合效率高等特点,大光敏面积的优势将扩展探测器在实际中的应用;也就是说,本发明的单光子探测器可实现高灵敏单光子探测,并具有探测面积大、速度快、制备简单,易于扩展到大规模阵列结构等特点;(1) The present invention provides an idea of structured superconducting strips to prepare large-area superconducting strip single-photon detectors. Through structural regulation, the sensitivity of the superconducting strips to photons is increased, and the cost of conventional superconducting single-photon detectors is reduced. Regarding the requirements for the width of superconducting strips, micron-wide structured superconducting strips allow the preparation of large photosensitive area detectors, which can achieve single photon detection while reducing the difficulty of process preparation. It has the characteristics of low preparation difficulty and high coupling efficiency. Large photosensitive The advantage of the area will expand the practical application of the detector; that is to say, the single-photon detector of the present invention can realize highly sensitive single-photon detection, and has the characteristics of large detection area, fast speed, simple preparation, and easy expansion to large-scale arrays Structural and other characteristics;
(2)与相同光敏面积下的超导纳米线单光子探测器相比,微米宽的结构化超导带单光子探测器具有更小的动态电感和恢复时间;在相同超导线宽度下,本发明中的结构化超导带的有效截面积更小,有助于提高探测器对单光子的响应能力;本发明的微米宽的结构化超导带具有较大的载流能力,这有助于读出端具有较大的信噪比;(2) Compared with superconducting nanowire single-photon detectors with the same photosensitive area, micron-wide structured superconducting strip single-photon detectors have smaller dynamic inductance and recovery time; under the same superconducting wire width, this The effective cross-sectional area of the structured superconducting strip in the invention is smaller, which helps to improve the response ability of the detector to single photons; the micron-wide structured superconducting strip in the invention has a larger current carrying capacity, which helps It has a large signal-to-noise ratio at the readout end;
(3)微米宽的结构化超导带具有较低的暗计数能力,有利于超导带单光子探测器在天文物理领域中的应用,如暗物质的探测。(3) Micron-wide structured superconducting strips have lower dark counting capabilities, which is beneficial to the application of superconducting strip single-photon detectors in the field of astronomy, such as the detection of dark matter.
附图说明Description of the drawings
图1是本发明结构化超导带单光子探测器的三维结构示意图;Figure 1 is a schematic three-dimensional structural diagram of the structured superconducting strip single photon detector of the present invention;
图2是本发明大光敏面积500×500μm 2的结构化超导带单光子探测器的全局SEM图; Figure 2 is a global SEM image of the structured superconducting strip single-photon detector with a large photosensitive area of 500×500 μm 2 of the present invention;
图3是本发明结构化超导带的局部SEM细节图;Figure 3 is a partial SEM detail view of the structured superconducting tape of the present invention;
图4是本发明结构化超导带单光子探测器的制备流程图;Figure 4 is a flow chart for the preparation of the structured superconducting strip single photon detector of the present invention;
图5是本发明结构化超导带单光子探测器在300mK工作温度下对光子响应的电压脉冲信号图;Figure 5 is a voltage pulse signal diagram of the structured superconducting strip single photon detector of the present invention responding to photons at an operating temperature of 300mK;
图6是本发明结构化超导带单光子探测器的电阻-温度曲线图;Figure 6 is a resistance-temperature curve of the structured superconducting strip single photon detector of the present invention;
图7是本发明结构化超导带单光子探测器在300mK工作温度下的电压-电流特性曲线;Figure 7 is the voltage-current characteristic curve of the structured superconducting strip single photon detector of the present invention at an operating temperature of 300mK;
图8是本发明结构化超导带单光子探测器在300mK工作温度下对1550nm波长的单光子计数和暗计数。Figure 8 shows the single photon counting and dark counting of the structured superconducting strip single photon detector of the present invention at a wavelength of 1550 nm at an operating temperature of 300 mK.
具体实施方式Detailed ways
现结合附图进一步阐述本发明实施例的技术方案。The technical solutions of the embodiments of the present invention will now be further described with reference to the accompanying drawings.
本发明实施例提出的结构化超导带单光子探测器,与几何热点破坏超导态类似,磁通穿越是超导薄膜发生相变的一种方法。通常,由于磁通势垒的存在,磁通在均匀的载流的超导薄膜中被有效钉扎。已有相关实验证明,超导带对单光子探测与磁通动力学有关,通过几何结构调控超导薄膜中的磁通运动有助于提高超导带对单光子的探测。本发明在微米宽的超导带上通过设计微纳孔阵列来实现结构化超导带,在本实施例中,微纳孔阵列以圆孔阵列为例子,具有圆孔阵列的结构化超导带可以促进磁通的产生和穿越。当入射光子被电流偏置的结构化超导带吸收后,热激发的磁通进入结构化超导带,导致 超导序参数(Δ)的局部抑制,一旦偏置电流超过一个阈值,阻止磁通穿越的势垒高度将减少为零。最终,磁通运动穿过整个超导薄膜,破坏了薄膜超导性并伴随一个可检测的电压脉冲,从而实现单光子探测。The structured superconducting strip single photon detector proposed in the embodiment of the present invention is similar to the geometric hot spot destroying the superconducting state. The magnetic flux crossing is a method for the phase change of the superconducting film. Typically, magnetic flux is effectively pinned in a uniform current-carrying superconducting film due to the presence of a magnetic flux barrier. Relevant experiments have proven that the detection of single photons by superconducting strips is related to magnetic flux dynamics. Controlling the movement of magnetic flux in superconducting films through geometric structures can help improve the detection of single photons by superconducting strips. The present invention realizes structured superconducting strips by designing micro-nanohole arrays on micron-wide superconducting strips. In this embodiment, the micro-nanohole array takes a circular hole array as an example. A structured superconducting strip with a circular hole array Strips can facilitate the generation and crossing of magnetic flux. When the incident photon is absorbed by the current-biased structured superconducting strip, the thermally excited magnetic flux enters the structured superconducting strip, resulting in local suppression of the superconducting order parameter (Δ). Once the bias current exceeds a threshold, the magnetic flux is prevented. The barrier height traversed by the pass will be reduced to zero. Eventually, the magnetic flux moves through the entire superconducting film, destroying the film's superconductivity and producing a detectable voltage pulse, enabling single-photon detection.
为了实现上述目的,本发明实施例的结构化超导带单光子探测器如图1所示,从下到上依次包括:衬底1、结构化超导带2、电极3、光学介质层4和光学反射层5。其中,结构化超导带2位于衬底1的表面上,电极3位于结构化超导带2的尾端连接处,光学介质层4位于结构化超导带2的表面上作为吸收光的增透层,光学反射层5位于光学介质层4的表面上,光学反射层5与光学介质层4构成探测器的光学腔来提高探测器对单光子的吸收效率。In order to achieve the above purpose, the structured superconducting strip single-photon detector according to the embodiment of the present invention is shown in Figure 1, which includes from bottom to top: substrate 1, structured superconducting strip 2, electrode 3, and optical medium layer 4 and optical reflection layer 5. Among them, the structured superconducting strip 2 is located on the surface of the substrate 1, the electrode 3 is located at the tail end connection of the structured superconducting strip 2, and the optical medium layer 4 is located on the surface of the structured superconducting strip 2 as an increaser for absorbing light. The transparent layer and the optical reflective layer 5 are located on the surface of the optical medium layer 4. The optical reflective layer 5 and the optical medium layer 4 constitute the optical cavity of the detector to improve the detector's absorption efficiency of single photons.
如图2和图3所示,结构化超导带2由超导MoSi薄膜组成,除了MoSi,还可以是MoGe、WSi、NbN、NbTiN薄膜,结构化超导带2的结构为首尾相连的蜿蜒的微米线,通过首尾相连的蜿蜒形状来提高探测器的填充率;在结构化超导带2上通过设计具有一定尺寸圆孔阵列结构来调控超导带的磁通的产生和穿越,有助于结构化超导带对单光子的探测。圆孔阵列中的参数,如孔的大小和间距是可以根据需求进行调控的。在一些实施例中,超导MoSi薄膜的厚度为4.5nm,超导带的宽度为1~3μm,超导带的填充率为0.3~0.7,圆孔直径为300nm,孔间距为200nm,探测器的光敏面积为500×500μm 2。由于超导带的宽度是微米量级的,相比于传统的纳米线,制备具有良好均匀性的大面积的结构化超导带单光子探测器更加容易,在实现单光子探测的同时,降低工艺制备难度。 As shown in Figures 2 and 3, the structured superconducting strip 2 is composed of a superconducting MoSi film. In addition to MoSi, it can also be a MoGe, WSi, NbN, or NbTiN film. The structure of the structured superconducting strip 2 is a meandering structure connected end to end. The meandering micron wires are connected end to end to improve the filling rate of the detector; on the structured superconducting strip 2, the generation and crossing of the magnetic flux of the superconducting strip are controlled by designing a circular hole array structure with a certain size. Contributes to the detection of single photons by structured superconducting strips. Parameters in the circular hole array, such as hole size and spacing, can be adjusted according to needs. In some embodiments, the thickness of the superconducting MoSi film is 4.5 nm, the width of the superconducting strip is 1 to 3 μm, the filling rate of the superconducting strip is 0.3 to 0.7, the diameter of the circular hole is 300 nm, and the hole spacing is 200 nm, and the detector The photosensitive area is 500×500μm 2 . Since the width of the superconducting strip is on the order of micrometers, compared with traditional nanowires, it is easier to prepare large-area structured superconducting strip single-photon detectors with good uniformity. While achieving single-photon detection, it reduces the cost Process preparation difficulty.
与超导纳米线单光子探测器相比,微米宽的结构化超导带具有较大的载流能力,这有助于外部电路读出端具有较大的信噪比;此外,在相同的光敏面积下,微米宽的结构化超导带单光子探测器具有更小的动态电感和恢复时间。以及光学介质层4和光学反射层5的存在可以提高结构化超导带对单光子的吸收率,从而提高超导带单光子探测器的探测效率。Compared with superconducting nanowire single-photon detectors, micron-wide structured superconducting strips have a larger current carrying capacity, which contributes to a larger signal-to-noise ratio at the external circuit readout; in addition, in the same Micron-wide structured superconducting strip single-photon detectors have smaller dynamic inductance and recovery time under the photosensitive area. And the existence of the optical medium layer 4 and the optical reflection layer 5 can increase the absorption rate of single photons by the structured superconducting strip, thereby improving the detection efficiency of the superconducting strip single photon detector.
本发明还提出了一种结构化超导带单光子探测器的制备方法,图4所示,包括以下步骤:The present invention also proposes a method for preparing a structured superconducting strip single photon detector, as shown in Figure 4, which includes the following steps:
S100:采用磁控溅射技术,在衬底1上生长超导MoSi薄膜;S100: Use magnetron sputtering technology to grow a superconducting MoSi film on substrate 1;
S200:通过紫外光刻、电子束蒸发和剥离技术在超导MoSi薄膜上生长一层具有一定图形的金电极;S200: Grow a layer of gold electrode with a certain pattern on the superconducting MoSi film through UV lithography, electron beam evaporation and lift-off technology;
S300:利用电子束曝光技术和反应离子刻蚀技术将具有圆孔阵列的结构化图形转移到超导MoSi薄膜上,得到具有圆孔阵列的结构化超导带2。S300: Using electron beam exposure technology and reactive ion etching technology to transfer the structured pattern with a circular hole array to the superconducting MoSi film, a structured superconducting strip with a circular hole array 2 is obtained.
S400:采用化学气相沉积技术在具有圆孔阵列的结构化超导带的表面上沉积一层纯二氧化硅,作为光学介质层4;S400: Use chemical vapor deposition technology to deposit a layer of pure silicon dioxide on the surface of a structured superconducting strip with a circular hole array as the optical medium layer 4;
S500:采用电子束蒸发和剥离技术在光学介质层4的表面上生成一层金属金(纯度 99.999%),作为光学反射层5。S500: Use electron beam evaporation and stripping technology to generate a layer of metallic gold (purity 99.999%) on the surface of the optical medium layer 4 as the optical reflective layer 5.
本发明的制备方法,可在超导薄膜上获得1~3μm超导带,超导带的填充率为0.5,其中超导带中心位置设计的圆孔阵列的直径为250~350nm,孔间距为200~300nm,探测器的光敏面积为500×500μm 2。这种几何调控超导带的制备工艺,有利于降低大面积超导带单光子探测器的制备难度,提高探测器的光敏面积,更宽的超导带具有探测近红外单光子的能力。 The preparation method of the present invention can obtain a 1-3 μm superconducting strip on a superconducting film. The filling rate of the superconducting strip is 0.5. The diameter of the circular hole array designed at the center of the superconducting strip is 250-350 nm, and the hole spacing is 200~300nm, the photosensitive area of the detector is 500×500μm 2 . This geometrically controlled superconducting ribbon preparation process is beneficial to reducing the difficulty of preparing large-area superconducting ribbon single-photon detectors and increasing the photosensitive area of the detector. Wider superconducting ribbons have the ability to detect near-infrared single photons.
现结合实施例进一步阐述本发明的制备方法。The preparation method of the present invention will be further described with reference to the examples.
本实施例的制备方法,包括以下步骤:The preparation method of this embodiment includes the following steps:
步骤1:对作为探测器衬底的双抛的热氧化硅衬底进行预处理,衬底还可以为石英、氧化镁、氟化镁和蓝宝石衬底,在本实施例中,选用厚度为268nm的双抛的热氧化硅衬底;本步骤的预处理包括:Step 1: Preprocess the double-polished thermal oxide silicon substrate as the detector substrate. The substrate can also be quartz, magnesium oxide, magnesium fluoride and sapphire substrate. In this embodiment, the thickness is 268nm. Double-polishd thermal oxidation silicon substrate; the preprocessing of this step includes:
先将双抛的热氧化硅衬底分别使用丙酮和乙醇在80W功率超声清洗以去除衬底表面的污染物,时间各5分钟;First, the double-polished thermally oxidized silicon substrate was ultrasonically cleaned with acetone and ethanol at 80W power for 5 minutes each to remove contaminants on the substrate surface;
再用去离子水进行冲洗;Then rinse with deionized water;
最后用氮气抢吹干衬底表面的水分。Finally, use nitrogen to blow dry the moisture on the surface of the substrate.
步骤2:采用磁控溅射技术在衬底上生长厚度为4.5nm的超导MoSi薄膜;具体实现步骤为:Step 2: Use magnetron sputtering technology to grow a superconducting MoSi film with a thickness of 4.5nm on the substrate; the specific implementation steps are:
将衬底送入磁控溅射的副室,并对衬底进行离子铣。离子铣条件为:15Sccm氩气流量、30mA离子束流、300V阳极电压,离子铣时间为1分钟。The substrate is sent into the auxiliary chamber of magnetron sputtering, and the substrate is ion milled. The ion milling conditions are: 15Sccm argon gas flow, 30mA ion beam current, 300V anode voltage, and the ion milling time is 1 minute.
将离子铣后的衬底送入磁控溅射的主室,并在主室的真空度为10 -6mTorr以下,在衬底上生长MoSi薄膜。MoSi薄膜的生长条件为:氩气流量为30Sccm、溅射气压为2mTorr、溅射电流0.5A、溅射速率为0.95nm/s。 The ion-milled substrate is sent into the main chamber of magnetron sputtering, and a MoSi film is grown on the substrate when the vacuum degree of the main chamber is below 10 -6 mTorr. The growth conditions of the MoSi film are: argon gas flow rate is 30Sccm, sputtering gas pressure is 2mTorr, sputtering current is 0.5A, and sputtering rate is 0.95nm/s.
在MoSi薄膜上原位生长一层Nb 5N 6薄膜作为保护层。Nb 5N 6薄膜生长条件为:氮气与氩气流量比为4:1、溅射气压为15mTorr、溅射功率为400W、溅射速率为0.2nm/s。 A layer of Nb 5 N 6 film was grown in situ on the MoSi film as a protective layer. The growth conditions of Nb 5 N 6 film are: nitrogen and argon flow ratio is 4:1, sputtering pressure is 15mTorr, sputtering power is 400W, and sputtering rate is 0.2nm/s.
步骤3:通过紫外光刻、电子束蒸发和剥离技术在超导MoSi薄膜上生长一层具有一定图形的金电极,金的厚度为120nm;具体操作步骤包括:Step 3: Grow a layer of gold electrode with a certain pattern on the superconducting MoSi film through UV lithography, electron beam evaporation and lift-off technology. The gold thickness is 120nm; specific operation steps include:
利用匀胶机在薄膜表面旋涂正性光刻胶AZ1500。Use a glue spreader to spin-coat positive photoresist AZ1500 on the film surface.
利用光刻机根据掩模版的图形对薄膜进行曝光。Use a photolithography machine to expose the film according to the pattern of the mask.
利用正性显影液对曝光后的薄膜进行显影,得到电极的图形。The exposed film is developed using a positive developing solution to obtain the electrode pattern.
利用电子束蒸发在显影后的薄膜上镀上一层金。Electron beam evaporation is used to coat the developed film with a layer of gold.
利用丙酮和乙醇在超声机上剥离多余的金。Use acetone and ethanol to peel off excess gold on an ultrasonic machine.
步骤4:利用电子束曝光技术和反应离子刻蚀技术将具有圆孔阵列的几何调控的形状转移到超导MoSi薄膜上;具体操作步骤包括:Step 4: Use electron beam exposure technology and reactive ion etching technology to transfer the geometrically controlled shape of the circular hole array to the superconducting MoSi film; specific operation steps include:
利用匀胶机在具有电极形状的超导MoSi薄膜表面旋涂厚度约为200nm的正性电子束抗蚀胶PMMA。本实施例中采用的PMMA的溶质浓度为4%,PMMA的前烘温度为180℃,烘烤时间为4min。The positive electron beam resist PMMA with a thickness of about 200nm is spin-coated on the surface of the superconducting MoSi film with an electrode shape using a glue leveler. The solute concentration of PMMA used in this embodiment is 4%, the pre-baking temperature of PMMA is 180°C, and the baking time is 4 minutes.
通过电子束曝光机采用2nA的电子束流绘制具有圆孔阵列的结构化超导带的图形;电子束曝光机的电子能量工作在100keV,曝光的束流为2nA,扫描步长为0.1~5nm,曝光剂量为600μC/cm 2。本实施例的具有圆孔阵列的结构化超导带的图形为:在超导带中心位置处排列圆孔形成具有圆孔阵列的超导带,孔的直径为250~350nm,孔间距为200~300nm,探测器的有效光敏面积为500×500μm 2The electron beam exposure machine uses an electron beam current of 2nA to draw the pattern of the structured superconducting strip with a circular hole array; the electron energy of the electron beam exposure machine works at 100keV, the exposure beam current is 2nA, and the scanning step is 0.1~5nm. , the exposure dose is 600μC/cm 2 . The pattern of the structured superconducting tape with a round hole array in this embodiment is: round holes are arranged at the center of the superconducting tape to form a superconducting tape with a round hole array. The diameter of the holes is 250-350 nm, and the hole spacing is 200 nm. ~300nm, the effective photosensitive area of the detector is 500×500μm 2 .
将曝光后的样品利用正胶显影液进行显影和定影处理,本实施例采用MIBK:IPA=1:3的混合液作为显影液,采用异丙醇作为定影液。显影时间为2分钟,定影时间为1分钟,在温度为22摄氏度的环境下操作。The exposed sample is developed and fixed using a positive film developer. In this example, a mixture of MIBK:IPA=1:3 is used as the developer, and isopropyl alcohol is used as the fixer. The development time is 2 minutes, the fixing time is 1 minute, and the temperature is 22 degrees Celsius.
利用反应离子刻蚀将显影后的具有圆孔阵列的结构化超导带图形转移至超导MoSi薄膜上;腔室气压为30mTorr、刻蚀速率为1nm/s。可根据薄膜厚度调整刻蚀时间。在本实施例中,反应离子刻蚀采用的气体为CF 4,流量为20Sccm,气压为1.2Pa,刻蚀功率为50W,刻蚀时间为90s。 Reactive ion etching was used to transfer the developed structured superconducting strip pattern with a circular hole array to the superconducting MoSi film; the chamber pressure was 30mTorr and the etching rate was 1nm/s. The etching time can be adjusted according to the film thickness. In this embodiment, the gas used for reactive ion etching is CF 4 , the flow rate is 20Sccm, the gas pressure is 1.2Pa, the etching power is 50W, and the etching time is 90s.
在水浴锅中利用N-甲基吡咯烷酮溶液除去残留在超导带表面的电子束光刻胶,水浴温度为80℃,水浴时间为30分钟~1小时。Use N-methylpyrrolidone solution in a water bath to remove the electron beam photoresist remaining on the surface of the superconducting strip. The water bath temperature is 80°C and the water bath time is 30 minutes to 1 hour.
最终获得了具有圆孔阵列的结构化超导带,如图2、3所示。Finally, a structured superconducting strip with a circular hole array was obtained, as shown in Figures 2 and 3.
步骤5:通过化学气相沉积技术在超导微米带上生长一层纯二氧化硅作为光学介质层,二氧化硅的厚度为268nm,有助于探测器对光子的吸收。Step 5: Use chemical vapor deposition technology to grow a layer of pure silicon dioxide on the superconducting micron strip as the optical medium layer. The thickness of the silicon dioxide is 268nm, which helps the detector absorb photons.
步骤6:通过光刻和电子束蒸发技术在光学介质层上生长一层金作为光学反射层,金的厚度为200nm。Step 6: Use photolithography and electron beam evaporation technology to grow a layer of gold as an optical reflective layer on the optical medium layer. The thickness of gold is 200nm.
本实施例制备得到的具有圆孔阵列的结构化超导带如图2、3所示,超导带宽度为1.5μm,填充率为0.5,超导带中心位置设计的圆孔阵列的直径为300nm,孔间距为200nm。图5所示为探测器的输出电压脉冲图,其中,探测器的恢复时间为149ns,脉冲幅度为310mV。图6所示为探测器的电阻随温度的变化曲线,从图可知,探测器的超导转变温度为3.6K。图7所示为探测器的电压-电流曲线,其超导临界电流为20μA。为了验证探测器的光学响应性能,对探测器在300mK的工作温度下,分别测量器件在1550nm单光子水平下的光子计数和暗计数,如图8所示。The structured superconducting strip with a circular hole array prepared in this embodiment is shown in Figures 2 and 3. The width of the superconducting strip is 1.5 μm, the filling rate is 0.5, and the diameter of the round hole array designed at the center of the superconducting strip is 300nm, pore spacing is 200nm. Figure 5 shows the output voltage pulse diagram of the detector, in which the recovery time of the detector is 149ns and the pulse amplitude is 310mV. Figure 6 shows the change curve of the detector's resistance with temperature. It can be seen from the figure that the superconducting transition temperature of the detector is 3.6K. Figure 7 shows the voltage-current curve of the detector, whose superconducting critical current is 20μA. In order to verify the optical response performance of the detector, the photon count and dark count of the device at the 1550nm single photon level were measured at the detector's operating temperature of 300mK, as shown in Figure 8.

Claims (9)

  1. 结构化超导带单光子探测器,其特征在于,所述探测器从下至上依次包括:衬底、位于所述衬底表面的结构化超导带、位于所述结构化超导带的尾端连接处的电极、位于所述结构化超导带表面的光学介质层和位于所述光学介质层表面的光学反射层;其中,所述结构化超导带是在超导带上设计具有微纳结构的图形,所述具有微纳结构的图形包括多个微纳孔结构,所述微纳孔结构为封闭形孔洞结构,所述封闭形孔洞结构包括但不限于圆孔、椭圆孔、方孔、矩形孔和和机翼孔。Structured superconducting strip single photon detector, characterized in that the detector includes from bottom to top: a substrate, a structured superconducting strip located on the surface of the substrate, and a tail located at the structured superconducting strip. The electrode at the end connection, the optical medium layer located on the surface of the structured superconducting tape and the optical reflective layer located on the surface of the optical medium layer; wherein, the structured superconducting tape is designed with microstructures on the superconducting tape. Patterns of nanostructures. The patterns with micro-nano structures include multiple micro-nano structures. The micro-nano structures are closed hole structures. The closed hole structures include but are not limited to round holes, elliptical holes, square holes, etc. holes, rectangular holes and wing holes.
  2. 根据权利要求1所述的结构化超导带单光子探测器,其特征在于,还包括:位于所述结构化超导带表面的光学介质层和位于所述光学介质层表面的光学反射层。The structured superconducting strip single photon detector according to claim 1, further comprising: an optical medium layer located on the surface of the structured superconducting strip and an optical reflection layer located on the surface of the optical medium layer.
  3. 根据权利要求1所述的结构化超导带单光子探测器,其特征在于,所述结构化超导带由超导薄膜组成,其结构为首尾相连的蜿蜒结构。The structured superconducting strip single photon detector according to claim 1, characterized in that the structured superconducting strip is composed of a superconducting film, and its structure is a meandering structure connected end to end.
  4. 根据权利要求1所述的结构化超导带单光子探测器,其特征在于,所述结构化超导带的宽度在0.1~20μm,超导带的填充率为0.1~0.9。The structured superconducting strip single photon detector according to claim 1, characterized in that the width of the structured superconducting strip is 0.1-20 μm, and the filling rate of the superconducting strip is 0.1-0.9.
  5. 根据权利要求1所述的结构化超导带单光子探测器,其特征在于,所述微纳孔结构的特征为沿着超导带方向的横向宽度为超导带宽度的3%~95%。The structured superconducting strip single photon detector according to claim 1, wherein the micro-nanohole structure is characterized by a lateral width along the superconducting strip direction of 3% to 95% of the superconducting strip width. .
  6. 结构化超导带单光子探测器的制备方法,其特征在于,包括以下步骤:A method for preparing a structured superconducting strip single photon detector, which is characterized by including the following steps:
    采用磁控溅射技术,在衬底上生长一层超导薄膜;Using magnetron sputtering technology, a layer of superconducting film is grown on the substrate;
    在超导薄膜上生长电极;Growing electrodes on superconducting films;
    采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到结构化超导带形状。Electron beam exposure technology and reactive ion etching technology are used to transfer the pattern of micro-nanopore structure to the superconducting film to obtain the shape of structured superconducting strips.
  7. 根据权利要求6所述的结构化超导带单光子探测器的制备方法,其特征在于,在所述采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到结构化超导带形状之后,还包括以下步骤:The method for preparing a structured superconducting strip single photon detector according to claim 6, wherein the pattern of the micro-nanopore structure is transferred to the superconducting film using electron beam exposure technology and reactive ion etching technology. After obtaining the structured superconducting strip shape, the following steps are also included:
    采用化学气相沉积法在具有微纳结构的超导带的表面上沉积一层二氧化硅作为光学介质层;A chemical vapor deposition method is used to deposit a layer of silicon dioxide as an optical medium layer on the surface of a superconducting strip with a micro-nano structure;
    采用电子束蒸发和剥离技术在光学介质层的表面上生长一层金作为光学反射层。Electron beam evaporation and lift-off techniques are used to grow a layer of gold on the surface of the optical medium layer as an optical reflective layer.
  8. 根据权利要求6所述的结构化超导带单光子探测器的制备方法,其特征在于,所述采用电子束曝光技术和反应离子刻蚀技术将微纳孔结构的图形转移到超导薄膜上,得到结构化超导带形状具体包括:The method for preparing a structured superconducting strip single photon detector according to claim 6, wherein the pattern of the micro-nano hole structure is transferred to the superconducting film using electron beam exposure technology and reactive ion etching technology. , obtaining the structured superconducting strip shape specifically includes:
    在具有电极的超导薄膜上旋涂正性电子束抗刻蚀胶作为电子束抗刻蚀层;Spin-coating the positive electron beam etching resist on the superconducting film with the electrode as the electron beam etching resisting layer;
    采用电子束曝光技术在具有电子束抗刻蚀层的薄膜上根据微纳结构的图形进行曝光,采用显影和定影处理在电子束抗刻蚀层上得到微纳结构的图形;Electron beam exposure technology is used to expose the film with an electron beam etching-resistant layer according to the pattern of the micro-nano structure, and development and fixing processes are used to obtain the pattern of the micro-nano structure on the electron beam etching-resistant layer;
    采用反应离子刻蚀技术将微纳孔结构的图形转移至薄膜上,得到具有结构化超导带形状;Reactive ion etching technology is used to transfer the pattern of micro-nanopore structure to the film to obtain a structured superconducting strip shape;
    利用N-甲基吡咯烷酮溶液水浴超声去除结构化超导带表面残留的正性电子束抗刻蚀胶,最终得到表面干净的结构化超导带。N-methylpyrrolidone solution water bath ultrasonic was used to remove the positive electron beam etching resist remaining on the surface of the structured superconducting tape, and finally a structured superconducting tape with a clean surface was obtained.
  9. 根据权利要求8所述的结构化超导带单光子探测器的制备方法,其特征在于:在电子束曝光技术中,采用2nA的电子束流在具有电子束抗刻蚀层的薄膜上绘制微纳结构的图形,曝光剂量为600μC/cm 2The method for preparing a structured superconducting strip single photon detector according to claim 8, characterized in that: in the electron beam exposure technology, an electron beam current of 2nA is used to draw microscopic particles on the film with an electron beam etching resistant layer. For the pattern of nanostructure, the exposure dose is 600μC/cm 2 .
PCT/CN2022/134848 2022-03-08 2022-11-29 Structured superconducting-tape single photon detector and preparation method therefor WO2023168996A1 (en)

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CN112885951A (en) * 2021-01-27 2021-06-01 电子科技大学 Porous superconducting niobium nitride nanowire and preparation method thereof
CN113257986A (en) * 2021-05-11 2021-08-13 中国科学院上海微系统与信息技术研究所 Superconducting nanowire single photon detector based on super-surface structure and preparation method thereof

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* Cited by examiner, † Cited by third party
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CN112885951A (en) * 2021-01-27 2021-06-01 电子科技大学 Porous superconducting niobium nitride nanowire and preparation method thereof
CN113257986A (en) * 2021-05-11 2021-08-13 中国科学院上海微系统与信息技术研究所 Superconducting nanowire single photon detector based on super-surface structure and preparation method thereof

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