EP3465725B1 - Méthode de fabrication d'une photocathode à nanofils - Google Patents

Méthode de fabrication d'une photocathode à nanofils Download PDF

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Publication number
EP3465725B1
EP3465725B1 EP17731230.3A EP17731230A EP3465725B1 EP 3465725 B1 EP3465725 B1 EP 3465725B1 EP 17731230 A EP17731230 A EP 17731230A EP 3465725 B1 EP3465725 B1 EP 3465725B1
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EP
European Patent Office
Prior art keywords
nanowires
photocathode
substrate
iii
growth
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EP17731230.3A
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German (de)
English (en)
French (fr)
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EP3465725A2 (fr
Inventor
Claude ALIBERT
Moustapha CONDE
Jean-Christophe Harmand
Théo JEGOREL
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Centre National de la Recherche Scientifique CNRS
Photonis France SAS
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Centre National de la Recherche Scientifique CNRS
Photonis France SAS
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J1/00—Details of electrodes, of magnetic control means, of screens, or of the mounting or spacing thereof, common to two or more basic types of discharge tubes or lamps
    • H01J1/02—Main electrodes
    • H01J1/34—Photo-emissive cathodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J9/00—Apparatus or processes specially adapted for the manufacture, installation, removal, maintenance of electric discharge tubes, discharge lamps, or parts thereof; Recovery of material from discharge tubes or lamps
    • H01J9/02—Manufacture of electrodes or electrode systems
    • H01J9/12—Manufacture of electrodes or electrode systems of photo-emissive cathodes; of secondary-emission electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J2201/00—Electrodes common to discharge tubes
    • H01J2201/34—Photoemissive electrodes
    • H01J2201/342—Cathodes
    • H01J2201/3421—Composition of the emitting surface
    • H01J2201/3423—Semiconductors, e.g. GaAs, NEA emitters
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
    • H01J40/00—Photoelectric discharge tubes not involving the ionisation of a gas
    • H01J40/02—Details
    • H01J40/04—Electrodes
    • H01J40/06—Photo-emissive cathodes

Definitions

  • the present invention relates to the field of photocathodes, in particular for electromagnetic radiation detectors such as image intensifiers or sensors of the EBCMOS (Electron Bombarded CMOS) or EBCDD (Electron Bombarded CDD) type.
  • electromagnetic radiation detectors such as image intensifiers or sensors of the EBCMOS (Electron Bombarded CMOS) or EBCDD (Electron Bombarded CDD) type.
  • Electromagnetic radiation detectors such as, for example, image intensifier tubes and photomultiplier tubes, detect electromagnetic radiation by converting it into a light or electrical output signal. They usually include a photocathode for receiving the electromagnetic radiation and emitting a flow of photoelectrons in response, an electron multiplier device for receiving said flow of photoelectrons and emitting in response a flow of so-called secondary electrons, then an output device for receiving said flow of secondary electrons and emit the output signal in response.
  • Photocathodes ensure the conversion of a flow of incident photons into a flow of photoelectrons. They are generally composed of a substrate transparent to the spectral band of interest and an electro-emissive layer deposited on the rear face of this substrate.
  • Photocathodes can be characterized by their quantum efficiency QE (Quantum Efficiency) defined as the average percentage of incident photons converted into photoelectrons or by their sensitivity defined as the photocathode current generated by a given luminous flux.
  • QE Quantum Efficiency
  • So-called second generation photocathodes use an electro-emissive layer of a multi-alkaline compound such as SbNaK or SbNa 2 KCs, deposited by CVD (Chemical Vapor Deposition) on a glass substrate.
  • the thickness of the photoemissive layer is usually between 50 and 200 nm.
  • the sensitivity of these photocathodes is generally 700 to 800 ⁇ A / lm and its quantum efficiency is relatively low (around 15%).
  • the so-called third generation photocathodes use an electro-emissive GaAs layer, epitaxied by MOCVD (Metal Organic Chemical Vapor Desposition) and transferred to a glass substrate.
  • the thickness of the electro-emissive layer is generally of the order of 2 ⁇ m.
  • the sensitivity of such a photocathode is of the order of 1500 to 2000 ⁇ A / lm.
  • Third generation photocathodes have high quantum efficiency, of the order of 30%, but their manufacturing is complex and expensive.
  • nanostructured photocathodes As described in the application WO-A-2003/043045 . These photocathodes are obtained by etching a pattern of channels in an alumina matrix and filling these channels, by an electrodeposition technique, with an electro-emissive material such as an alkaline compound or a III-V semiconductor.
  • photocathodes can achieve high sensitivities but are complex to manufacture.
  • the transfer of the emissive layer onto a transparent substrate at the spectral band of interest turns out to be particularly delicate due to the fragility of the nanostructure.
  • the nanostructure is directly etched in a substrate constituting the input window of the photocathode, a significant part of the conversion takes place in the massive part of the semiconductor layer so that the quantum yield is reduced by the recombinations within it.
  • the aim of the present invention is therefore to provide a method of manufacturing a photocathode with high sensitivity levels/quantum efficiency.
  • the present invention is defined by a photocathode manufacturing method as given in claim 1.
  • Advantageous embodiments are given in the dependent claims.
  • the present invention is based on the surprising observation that it is possible, under certain conditions, to directly epitaxy III-V semiconductor nanowires with high crystalline quality on an amorphous substrate such as a glass substrate.
  • an amorphous substrate such as a glass substrate.
  • the research carried out to date in terms of nanowire growth focused either on crystalline substrates or on amorphous substrates undergoing a prior surface crystallization step.
  • FIG. 1A schematically represents a first nanowire photocathode structure, which can be produced by a manufacturing method according to the invention.
  • the photocathode comprises an amorphous substrate such as a glass substrate, 110, constituting the input window of the image intensifier or sensor.
  • the amorphous substrate material is chosen to be transparent in the working spectral band of the photocathode. If necessary, the amorphous substrate can be nano-structured to allow a more regular distribution of the nanowires at the cost of greater complexity. Growth then begins in the wells of the nanostructure.
  • the substrate is covered with a mat of nanowires made of III-V semiconductor material, for example GaN, InGaN, InGaAs, GaP, InGaP, InAs, GaSb, GaAsSb, AlGaAS, AlGaASP, GaBiAs and more generally their ternary and quaternary alloys.
  • III-V semiconductor material for example GaN, InGaN, InGaAs, GaP, InGaP, InAs, GaSb, GaAsSb, AlGaAS, AlGaASP, GaBiAs and more generally their ternary and quaternary alloys.
  • the nanowires are doped with a P-type material, for example Zn, Be, C, or an amphoteric material such as Si.
  • a P-type material for example Zn, Be, C, or an amphoteric material such as Si.
  • the nanowire mat, 120 is grown directly on the amorphous substrate by molecular beam epitaxy (MBE), as described later.
  • MBE molecular beam epitaxy
  • the nanowires have a diameter of 20 to 500 nm, preferably between 50 to 150 nm.
  • the nanowire mat has a density of 10 5 to 10 10 cm -2 , preferably 10 8 to 10 9 cm -2 .
  • a metal layer, 130 acts as an electrode and makes it possible to apply polarization to the mat of nanowires.
  • This polarization is negative with respect to a distant anode (not shown), opposite the photocathode.
  • the photons arriving on the entrance face of the substrate, transparent at the wavelength of interest generate electron-hole pairs within the nanowires.
  • the holes are eliminated by recombination with the electrons provided by the polarization electrode, 130.
  • the electrons generated can be emitted over the entire length of the nanowires.
  • the nanowires are covered with a layer intended to lower the work function, for example in LiO, CsO or NF 3 and therefore to facilitate the extraction of electrons in a vacuum.
  • the electrons extracted from the nanowires can then be multiplied by an electron multiplier, 140, such as a wafer of microchannels or a layer of nanodiamonds (NDs).
  • the secondary electrons thus generated can then form an image on a phosphorescent screen or on a matrix of CMOS transistors or even a CCD matrix (EBCCD), in a manner known per se.
  • the electrons extracted from the nanowires can directly impact the rear face of an EBCMOS (Electron Bombarded CMOS) sensor.
  • EBCMOS Electro Bombarded CMOS
  • the phosphor screen, the CCD, CMOS or EBCMOS matrix constitute the output window of the detector.
  • FIG. 1B schematically represents a second structure of a nanowire photocathode, which can be produced by a manufacturing method according to the invention.
  • the elements identical to those of the Fig. 1A bear the same reference numbers and will not be described again.
  • This second structure differs from the first by the presence of a contact layer, 135, transparent in the spectral band of interest and conductive, for example, an ITO layer, a graphene layer, or even a thin polycrystalline layer of heavily P-doped III-V semiconductor material, deposited on the substrate before the growth of the nanowire mat.
  • the contact layer, 135, is electrically connected to the polarization electrode, 130.
  • FIG. 1 C schematically represents a third structure of a nanowire photocathode which can be produced by a manufacturing method according to the invention.
  • the elements identical to those of the Fig. 1B bear the same reference numbers and will not be described again.
  • This third structure differs from the previous one by the presence of an anti-reflection layer, 125.
  • This anti-reflection layer is deposited on the surface of the substrate before the deposition of the contact layer, 135. It prevents light from entering the strip working spectral of the photocathode is reflected by the interface between the substrate, 110, and the contact layer, 135.
  • FIGs. 1A to 1C illustrate photocathode structures operating in transmission in the sense that they are located between the input window and the output window of the detector.
  • these photocathodes can operate in reflection. More precisely, the flow of photons is in this case incident on the rear face of the photocathode (with an angle of incidence determined by input optics) and the photoelectrons generated in the nanowires are emitted by this same rear face.
  • the entrance and exit windows of the detector are therefore located here on the same side of the photocathode.
  • amorphous substrate such as a glass substrate
  • an anti-reflective layer and a contact layer will be described below.
  • the growth of the nanowires is carried out by molecular beam epitaxy (MBE) of the III-V semiconductor material on the amorphous substrate.
  • MBE molecular beam epitaxy
  • a gold film is first deposited on the substrate.
  • the gold is deposited at a temperature between 800 and 1200°C (temperature of the MBE cell) on the ambient or hot substrate, preferably between 400°C and 700°C, for a period of 1 to 30 min.
  • At the end of the deposition of the gold film we wait for a period of 30 seconds to 30 minutes, so that the gold dewets on the substrate.
  • Gold particles 5 to 50nm in diameter are then formed on the glass substrate.
  • a colloidal solution of gold particles having the aforementioned size can be dispersed on the surface of the substrate. In all cases, the gold particles act as precursors for the growth of III-V material nanowires.
  • the gold film is deposited or dispersed on the contact layer.
  • the dewetting and nucleation phenomenon is essentially the same as on the glass substrate.
  • the growth of the nanowires is then carried out in the same MBE frame, which avoids any contamination by ambient air. It is carried out in a temperature range of 400 to 700°C. The temperature is measured using a pyrometer adapted to the wavelength of the III-V materials making up the nanowires.
  • the atomic fluxes are chosen to correspond to growth rates between 0.5 ⁇ /s and 10 ⁇ /s.
  • the flows are calibrated by high energy electron diffraction at grazing incidence or RHEED ( Reflection High Energy Electron Diffraction ) by observing the RHEED observations corresponding to the deposition of successive layers, in a manner known per se. After a few seconds of growth, the diffraction pattern shows semicircles indicating the growth of single-crystal nanowires in a multitude of directions.
  • FIG. 2 represents a photograph obtained by scanning electron microscopy (SEM) of a mat of GaAs nanowires having grown by MBE epitaxy on a glass substrate (Corning TM 7056).
  • the flow ratio of the III-V materials during growth so that the nanowires have a wider band gap at their base (and at their periphery) than at their top (and in their hearts).
  • This variation in composition can be carried out in stages over time. Alternatively, it could be gradual so as to obtain a positive band gap gradient directed from the core of the nanowires towards their periphery.
  • this variant will make it possible to absorb a wider spectral band than with a simple homogeneous composition.
  • an activation layer of LiO, CsO or NF 3 At the end of the growth of the nanowires, in the same frame or without breaking the ultra-high vacuum, we can advantageously deposit an activation layer of LiO, CsO or NF 3 .
  • the electrons generated in the nanowires have a high probability of being emitted into a vacuum before being recombined.
  • the emission of photoelectrons can take place all along the nanowires. What's more, the high electric field due to the tip effect also increases the emission probability compared to a conventional planar photocathode configuration.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Common Detailed Techniques For Electron Tubes Or Discharge Tubes (AREA)
EP17731230.3A 2016-05-31 2017-05-29 Méthode de fabrication d'une photocathode à nanofils Active EP3465725B1 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR1654896A FR3051963B1 (fr) 2016-05-31 2016-05-31 Photocathode a nanofils et methode de fabrication d'une telle photocathode
PCT/FR2017/051321 WO2017207898A2 (fr) 2016-05-31 2017-05-29 Photocathode à nanofils et méthode de fabrication d'une telle photocathode

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EP3465725A2 EP3465725A2 (fr) 2019-04-10
EP3465725B1 true EP3465725B1 (fr) 2023-09-27

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US (1) US11043350B2 (zh)
EP (1) EP3465725B1 (zh)
JP (1) JP7033556B2 (zh)
KR (1) KR102419131B1 (zh)
FR (1) FR3051963B1 (zh)
IL (1) IL263234B2 (zh)
TW (1) TWI747907B (zh)
WO (1) WO2017207898A2 (zh)

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CN108281337B (zh) * 2018-03-23 2024-04-05 中国工程物理研究院激光聚变研究中心 光电阴极及x射线诊断系统
JP6958827B1 (ja) * 2020-05-20 2021-11-02 国立大学法人静岡大学 光電陰極及び光電陰極の製造方法
CN112530768B (zh) * 2020-12-21 2024-02-27 中国计量大学 一种高量子效率的纳米阵列光电阴极及其制备方法
CN113964003A (zh) * 2021-10-09 2022-01-21 电子科技大学长三角研究院(湖州) 一种具有纳米管结构的GaN光电阴极及其制备方法

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JP2001143648A (ja) 1999-11-17 2001-05-25 Hitachi Ltd 光励起電子線源および電子線応用装置
US6908355B2 (en) * 2001-11-13 2005-06-21 Burle Technologies, Inc. Photocathode
JP2006302610A (ja) 2005-04-19 2006-11-02 Hamamatsu Photonics Kk 半導体光電陰極
JP2008135350A (ja) 2006-11-29 2008-06-12 Hamamatsu Photonics Kk 半導体光電陰極
US20100180950A1 (en) * 2008-11-14 2010-07-22 University Of Connecticut Low-temperature surface doping/alloying/coating of large scale semiconductor nanowire arrays
JP5437487B2 (ja) * 2010-06-03 2014-03-12 ｎｕｓｏｌａ株式会社 光蓄電装置
WO2012067687A2 (en) 2010-08-26 2012-05-24 The Ohio State University Nanoscale emitters with polarization grading
WO2013126432A1 (en) * 2012-02-21 2013-08-29 California Institute Of Technology Axially-integrated epitaxially-grown tandem wire arrays
CN103594302B (zh) * 2013-11-19 2016-03-23 东华理工大学 一种GaAs纳米线阵列光电阴极及其制备方法
US9478385B2 (en) * 2013-11-26 2016-10-25 Electronics And Telecommunications Research Institute Field emission device having field emitter including photoelectric material and method of manufacturing the same
CN104752117B (zh) * 2015-03-03 2017-04-26 东华理工大学 一种垂直发射AlGaAs/GaAs纳米线的NEA电子源
CA2923897C (en) * 2015-03-16 2023-08-29 Zetian Mi Photocathodes and dual photoelectrodes for nanowire photonic devices
FR3034908B1 (fr) 2015-04-08 2017-05-05 Photonis France Photocathode multibande et detecteur associe
US9818894B2 (en) * 2015-09-02 2017-11-14 Physical Optics Corporation Photodetector with nanowire photocathode

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Publication number Publication date
JP2019523522A (ja) 2019-08-22
IL263234A (en) 2018-12-31
US20200328056A1 (en) 2020-10-15
KR20190013800A (ko) 2019-02-11
JP7033556B2 (ja) 2022-03-10
US11043350B2 (en) 2021-06-22
EP3465725A2 (fr) 2019-04-10
TWI747907B (zh) 2021-12-01
IL263234B2 (en) 2023-08-01
KR102419131B1 (ko) 2022-07-08
TW201810695A (zh) 2018-03-16
WO2017207898A3 (fr) 2018-01-25
IL263234B1 (en) 2023-04-01
FR3051963A1 (fr) 2017-12-01
FR3051963B1 (fr) 2020-12-25
WO2017207898A2 (fr) 2017-12-07

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