Classifications

• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
  • H01J37/02—Details
  • H01J37/04—Arrangements of electrodes and associated parts for generating or controlling the discharge, e.g. electron-optical arrangement, ion-optical arrangement
  • H01J37/06—Electron sources; Electron guns
  • H01J37/073—Electron guns using field emission, photo emission, or secondary emission electron sources
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J3/00—Details of electron-optical or ion-optical arrangements or of ion traps common to two or more basic types of discharge tubes or lamps
  • H01J3/02—Electron guns
  • H01J3/021—Electron guns using a field emission, photo emission, or secondary emission electron source
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2203/00—Electron or ion optical arrangements common to discharge tubes or lamps
  • H01J2203/02—Electron guns
  • H01J2203/0204—Electron guns using cold cathodes, e.g. field emission cathodes
  • H01J2203/0292—Potentials applied to the electrodes
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2203/00—Electron or ion optical arrangements common to discharge tubes or lamps
  • H01J2203/04—Ion guns
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/06—Sources
  • H01J2237/061—Construction
  • H01J2237/062—Reducing size of gun
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/06—Sources
  • H01J2237/063—Electron sources
  • H01J2237/06325—Cold-cathode sources
  • H01J2237/06333—Photo emission
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/06—Sources
  • H01J2237/08—Ion sources
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
  • H01J2237/00—Discharge tubes exposing object to beam, e.g. for analysis treatment, etching, imaging
  • H01J2237/26—Electron or ion microscopes
  • H01J2237/2602—Details
  • H01J2237/2605—Details operating at elevated pressures, e.g. atmosphere

Definitions

• the invention lies in the field of generators of electrically charged particles for chemical, physical-chemical or biology analyzes.
• An object of the invention is a pulsed generator of electrically charged particles capable of generating packets of particles having a temporal duration less than or equal to 1 nanosecond or even less than or equal to 5 picoseconds according to one embodiment of the invention, or even less than or equal at 100 femtoseconds.
• the generator according to the invention is capable of producing packets of electrons or ions.
• the applications of the device according to the invention concern all areas of electron-matter interaction: characterizations by diffraction (LEED, RHEED, gas phase, nano-objects, UED), studies of surface physics, Auger spectroscopy, experiments and sources ionization (aerosols, mass spectrometry), hardening of materials, irradiations (scintillator tests, simulation irradiations, micro-fabrication, biological materials), NDT, analysis of contaminants, microscopy, electron-induced desorption.
• Another object of the invention is a method of using the charged particle generator according to the invention.
• a first family is that of Accelerator or High Energy Physicists. It develops robust and very heavy equipment, the dimensions of which are important.
• the particles obtained are very energetic, in continuous train or in packets of numerous particles, at a high repetition rate (300 GHz). These particles are not used, because they do not come out of the ring, but they are used to produce photons.
• the free electron laser or XFEL according to the English translation X-ray Free Electron Laser is a machine which tends to replace synchrotrons and which is also available to users of photons.
• the repetition rates are 25 to 50 MHz due to the complexity of the events to be detected and the operation of the detectors.
• the document “A pulsed electron gun for ultrafast electron diffraction at surfaces” by A. Janzen et al. published in “Review of Scientific Instruments” N. 78 in 2007 discloses an electron gun for the analysis of surfaces by electron beams. This device makes it possible to maintain the ultra-high vacuum required for the targeted application. In this gun, the cathode and the anode are as spaced as possible so as to minimize the risk of electrical breakdown and the focusing of the electron beam is carried out using electrostatic lenses.
• the document “Intrinsic Emittance Reduction of an Electron Beam from Metal Photocathodes” by CP Hauri et al. published in “Physical Review Letters” N. 104 in 2010 discloses the use of various metal conversion targets such as Mo, Nb or AI usually used in high energy physics. However, this document refers exclusively to large size devices.
• the second family is that of the Physicists of Optics. It naturally uses a primary laser source and a conversion target, usually metallic or semiconducting, but also plasma. It is often pulsed, at a recurrence rate of 10 Hz to a few MHz, but always fixed. The realizations strive to obtain significantly smaller particle packets than for the first family, in order to reduce the space charge. For this family, the main objective displayed is the race to obtain the ultimate duration of the particle bunch (from a hundred attoseconds to a hundred femtoseconds), without considerations for the degree of vacuum, simplicity or comfort in use. The energies involved may be lower than those of the first family, but the target beam energies are generally 30 keV to 200 MeV.
• the electron guns can be pulsed in mono-electronic mode but not necessarily (they can deliver packets of several tens of thousands of electrons, like the 1 st family), the distances are in decimeters or in meters and high vacuum or ultra high vacuum is required.
• the third technological family is that of physical chemists. It strives to produce particles energetic enough to ionize matter, but does not control the primary source. It aims to place the sample as close as possible to particle production and does not necessarily seek high vacuum or ultra high vacuum for its applications.
• the instruments thus developed have low temporal resolutions and ill-defined energies. When these two parameters become important for studies, physical chemists must resort to instruments from the first family.
• a fourth technological family is that of the Physicists of Electron Microscopy. This can be illustrated by document WO 2010/042629 A2, which aims to make a thermionic source and a source of photons co-operate in an electron microscope from modulating the emission of the 1 st source.
• Document DE 10245052 A1 relates to an electron microscope, but the electron source of which is produced according to the techniques of the second family with a train of electron packets chopped attosecond by interaction with an ultra-laser. fast. The whole is under ultra-vacuum with electrostatic focusing lenses.
• the Applicant has also developed an electron gun capable of generating packets of particles by photoelectric emission.
• This device called LUBIOL, has a vacuum chamber with a very low operating pressure of the order of 10 7 mbar.
• the electron packets contain a high number of particles and of the order of 10 3 .
• the kinetic energy of the electrons is of the order of keV with a repetition rate of the order of kHz.
• An electrostatic lens system is used to maintain these characteristics of the electron beam at the sample level.
• This system has a certain number of drawbacks, in particular the impossibility of overcoming the high vacuum, ie of increasing the operating pressure, the impossibility of extracting the beam in the presence of a gaseous atmosphere, the impossibility of working with fragile or liquid or desorbent samples, the impossibility of reducing the dimensions of the system and the impossibility of obtaining a robust and easy-to-use instrument.
• state-of-the-art electrically charged particle generators have constraints that prevent their use for the analysis of certain samples. For example, devices that require a high vacuum do not allow the analysis of biological, liquid or desorbent samples. In addition, the systems which allow a high operating pressure and therefore compatible with fragile samples, have a low temporal and energy resolution.
• the invention aims to provide an ultra-fast pulsed source of electrically charged particles which is portable, therefore having dimensions and energy consumption as low as possible, and which has a temporal resolution of the order of a picosecond, while destroying as little as possible fragile samples, such as liquid or biological samples.
• the invention relates to a pulsed generator of electrically charged particles comprising:
• the vacuum chamber is configured to maintain an internal operating pressure of between 10 6 mbar and atmospheric pressure; the vacuum chamber is configured to accommodate a photocathode and an anode, the photocathode and the anode being separated by an adjustable distance less than or equal to 30 mm, preferably less than or equal to 20 mm;
• the vacuum enclosure has an optical window allowing pulsed light to first reach a rear face of the photocathode;
• the anode is arranged downstream of the photocathode and has an orifice suitable for the passage of electrically charged particles;
• said pulsed generator of electrically charged particles comprises means for applying a potential difference between the photocathode and the anode, said potential difference being configured to accelerate the charged particles.
• Electrically charged particles are understood to mean electrons or ions intended for the chemical, physico-chemical or biological analysis of a sample to be characterized.
• Upstream and downstream are understood to mean the position of a part relative to the direction of a light beam emitted by a pulsed light source. Likewise, the front of a room is the side where the light beam comes in and the back is the other side.
• the generator initially produces electrons which are optionally converted into ions by interaction with an appropriate medium.
• the generator according to the invention makes it possible to produce packets of charged particles having an ultra-short time duration, for example less than or equal to 5 picoseconds (ps).
• the packets generated comprise a small number of charged particles, or even a single charged particle. More generally, the invention makes it possible to obtain packets of charged particles having a temporal duration less than or equal to 1 nanosecond (ns) or even less than or equal to 5 picoseconds according to one embodiment of the invention, or even less than or equal to 100 femtoseconds (fs).
• pulsed light source is meant a light source capable of providing pulses of light.
• the pulsed light source is a laser providing pulses of the duration of 120 fs with a repetition rate of 80 MHz or of duration 100 fs with a repetition rate of 100 MHz.
• the pulses have an average wavelength centered in the ultraviolet, for example around 266 nm.
• the light used is incoherent light, such as a pulsed LED emitting pulses having a temporal duration less than or equal to 70 picoseconds.
• vacuum chamber means a device for maintaining an internal pressure less than or equal to atmospheric pressure.
• the vacuum chamber is further configured to accommodate the elements needed to produce the charged particle packets.
• the vacuum chamber is configured to also accommodate the sample to be characterized.
• the vacuum chamber is provided with a window transparent to the charged particles and placed on the axis of their exit path from the chamber, and the sample is placed on this path at the exterior of the enclosure, preferably as close as possible to it.
• the vacuum chamber is configured to maintain an operating pressure between 10 6 mbar and atmospheric pressure.
• the device according to the invention can be configured to work at an operating pressure of between 10 3 mbar and atmospheric pressure, which allows the analysis of fragile, liquid or biological samples. This analysis is carried out using a diagnostic module.
• photocathode is understood to mean an electrode intended to emit electrons by photoelectric effect or photoelectrons. Photoelectrons are obtained by sending the pulsed light to the photocathode. According to one embodiment, the photocathode is metallic.
• the photocathode is backlit thus the electrons are emitted from the downstream side of the photocathode and therefore in the same direction as the photons of the light beam.
• the electrons emitted at the exit of the photocathode are it at a very low speed, they are then accelerated by bringing the photocathode to a potential of 0 to -30 kV, the anode being at potential 0.
• the orifice on the anode allows the passage of electrically charged particles accelerated by the potential difference applied between the photocathode and the anode.
• the charged particles leaving the anode can then be sent to a sample to be analyzed.
• optical window is meant an optical element allowing the pulsed light to reach the photocathode.
• the optical window can for example comprise a window, an optical fiber passage, a lens or a combination of these elements.
• the optical window is sealed, ensuring that the working pressure is maintained inside the vacuum chamber.
• the optical window is directly the entry face of the photocathode.
• the distance between cathode and anode is adjustable, which makes it possible to adapt the maximum energy that can be given to the particles without breakdown.
• this makes it possible to obtain a very compact device depending on the applied voltage.
• the distance L between the photocathode and the anode has a value of 300 ⁇ m for a bias voltage of the photocathode of 1 kV, or even 5 kV.
• the voltage is limited to 5kV, there is no radioactive risk since the energies of the electron beams generated are in the range 1 -5 keV.
• energies up to 5 keV we benefit from an exemption on radiation protection (cf. Art. R. 4451-1 and Article L. 1333-1 of the public health code).
• this distance is increased by a proportional factor of 2, 4 or 6, or even 10, 20 or 30 to avoid electrical breakdown, but the size of the device remains of the order of magnitude of 10 mm which is much less than the prior art.
• the reduction of the distance between the photocathode and the anode allows a higher operating pressure inside the vacuum chamber.
• the particle generator according to the invention operates with a higher working pressure than the particle generators of the state of the art. This makes it possible to analyze biological or liquid samples that are not compatible with vacuum or ultra-vacuum.
• the sample to be characterized can be placed inside the vacuum chamber and closer to the anode than in the prior art. This makes it possible to reduce the distance between the anode and the sample to be analyzed and therefore to reduce the effects of temporal dispersion of packets of charged particles.
• the generator according to the invention makes it possible to obtain packets of charged particles with very short time durations of less than 5 picoseconds, or even less than a picosecond.
• the charged particle generator according to the invention therefore makes it possible to analyze fragile samples such as liquid or biological samples with a very high temporal resolution, which is not possible with the devices known from the skilled in the art.
• the generator according to the invention has small dimensions and low energy consumption.
• the samples to be analyzed do not withstand a pressure lower than atmospheric pressure, one can resort to the variant of the invention comprising a window transparent to the charged particles and located in their path. The sample is then placed against this window while being outside the vacuum chamber. If the sample is liquid, the generator according to the invention can be oriented so that the beam exits from the top, the particle exit window then being horizontal.
• the window transparent to the charged particles may be absent, and in this case the generator is directly coupled to an existing vacuum chamber.
• the photocathode comprises an Au film, and a Cr or Ti bond film which allows a much longer service life without maintenance under degraded vacuum conditions than the photocathodes used.
• the invention can use this type of photocathode with Au film, neglected by those skilled in the art, because of the choice deliberate low number of electrons per pulse, which is compensated by the fact that these pulses are renewed at high rate.
• the elements present inside the vacuum chamber are obtained by depositing thin or ultra-thin layers on blades having an optical quality polish. This allows the application of electric fields with intensities greater than 30 MV / m while reducing the risk of electrical breakdown.
• the charged particle generator according to the invention further comprises means for modifying the direction of the pulsed light beam, so as to modify the point and the angle of attack of the photocathode.
• the generator according to the invention makes it possible to modify the point of focus of the light beam as well as its angle of arrival at the photocathode.
• the generator according to the invention further comprises a breakdown detector.
• the breakdown detector makes it possible to determine, for a given electric field, the electrical breakdown pressure. It is therefore possible to choose a high working pressure while avoiding electrical breakdown.
• the device according to the invention avoids electrical breakdown not by a higher vacuum as in the prior art, but on the contrary by a little marked vacuum, or even almost non-existent associated with a breakdown detector consisting of a spark gap adjusted to a voltage slightly lower than the breakdown voltage of the device, and giving a warning signal allowing the operating conditions (vacuum chamber pressure or anode-cathode distance) to be slightly deviated from the operating conditions. breakdown.
• the device according to the invention makes it possible to generate packets of particles having a temporal duration less than or equal to 1 nanosecond or even less than or equal to 5 picoseconds according to one embodiment of the invention, or even less than or equal to 100 femtoseconds. .
• the photocathode is brought to a negative potential, the anode is at a zero potential, like the sample, it is therefore possible in certain cases to consider having a zero distance between the anode and the 'sample, but in general we will put a spacer between the two so as not to damage the sample, but it can be very thin. It is possible to have the photocathode at zero potential and the anode at a potential> 0 but this would be dangerous both for the user and for the sample and could induce short circuits.
• the distance between the photocathode and the sample does not play much on the temporal resolution (within a few fs) in the vicinity of breakdown conditions.
• the table below shows, for photocathode and anode voltages and distances, the acceleration field obtained and the electron packet durations obtained at 25 mm from the photocathode, knowing that we are trying to stay around from 3 kV.mnr 1 to 10 5 mbar so as not to have breakdown, around 1.5 kV.rmnr 1 to 10 4 mbar etc.
• the distance between the photocathode and the anode is less than 10 mm;
• the distance between the photocathode and the anode is less than 2 mm;
• the polarization voltage of the photocathode is less than or equal in absolute value to 30 kV (preferably between -30 kV and 0V) so as to obtain packets of electrically charged particles, each packet having a time duration less than or equal to 5 ps;
• the polarization voltage of the photocathode is less than or equal in absolute value to 10 kV (preferably between -10 kV and 0V) so as to obtain packets of electrically charged particles, each packet having a time duration less than or equal to 5 ps;
• the polarization voltage of the photocathode is less than or equal in absolute value to 5 kV (preferably between -5 kV and OV) and the distance between photocathode and anode is less than or equal to 1.5 mm, preferably less than or equal at 300 ⁇ m;
• the polarization voltage of the photocathode is less than or equal in absolute value to 10 kV (preferably between -10 kV and 0V) and the distance between photocathode and anode is less than or equal to 3 mm, preferably less than or equal to 600 pm;
• the polarization voltage of the photocathode is less than or equal in absolute value to 20 kV (preferably between -20 kV and 0V) and the distance between photocathode and anode is less than or equal to 6 mm, preferably less than or equal to 1 , 2 mm;
• the polarization voltage of the photocathode is less than or equal in absolute value to 30 kV (preferably between -30 kV and 0V) and the distance between photocathode and anode is less than or equal to 10 mm, preferably less than or equal to 1 , 8 mm;
• the pulsed light source produces light pulses having a temporal duration less than or equal to 5 ps;
• the generator further comprises a breakdown detector
• the breakdown detector is placed near the anode and includes:
• the breakdown detector is configured to determine the electrical breakdown pressure under the bias voltage of the photocathode used;
• the sample to be analyzed is placed inside or outside the vacuum chamber;
• the pulsed generator includes a diagnostic module for analyzing the sample.
• the sample to be analyzed is at a distance d2 from the diagnostic module such that 0 ⁇ d2 ⁇ 60 mm when the sample is placed outside and d1 is such that 0 ⁇ d2 ⁇ 0.7 mm when the sample is placed inside.
• the generator according to the invention has in the axis of the beam of charged particles a window transparent to said charged particles and making it possible to maintain a pressure below atmospheric pressure in the enclosure;
• the window transparent to charged particles is a membrane, which is particularly suitable if the sample is of low density such as a gas or if it is a liquid;
• the membrane is made of silicon nitride S13N4 or of graphene (C) n and has a thickness of between a few nm and a few hundred nm, typically between 2 and 200 nm;
• the photocathode comprises a metallic nanometric stack on a thin optical plate type substrate;
• the orifice of the anode is anisotropic and has a first characteristic dimension and a second characteristic dimension, the second characteristic dimension being at least twice as large as the first characteristic dimension; the two characteristic dimensions are mutually orthogonal and both orthogon
• the generator further comprises another diagnostic module for determining the temporal duration of the packets of electrically charged particles;
• the breakdown detector is configured to provide an alert signal and / or stop the particle generator if the operating pressure inside the vacuum chamber is not low enough to avoid the risk of electrical breakdown;
• the charged particles are ions and the generator according to the invention further comprises the following elements: a gas capable of emitting positive ions during electron bombardment; at least one anode for focusing the ion beam.
• Another object of the invention is a method of using the pulsed generator of charged particles according to the invention.
• the method according to the invention allows, according to a first mode of use, the analysis of a sample using a pulsed generator of charged particles according to the invention and comprising the following steps: placing the sample in the vacuum chamber, placing the vacuum chamber under vacuum between 10 6 mbar, preferably 10 5 mbar, and atmospheric pressure; placing the pulsed charged particle generator on a table in front of a pulsed light source; positioning of a diagnostic module for the analysis of the sample in the downstream position of the sample.
• the module D ’ is placed in the vacuum chamber.
• the module D ’ is placed outside the vacuum chamber.
• the method according to the invention allows according to a second mode of use, the analysis of a sample using a pulsed generator of charged particles according to the invention and comprising the following steps: placing the enclosure under vacuum at vacuum between 10 6 mbar, preferably 10 5 mbar, and atmospheric pressure; placing the pulsed charged particle generator on a table in front of a pulsed light source; placement of the sample in the downstream position of the vacuum chamber, positioning of a diagnostic module for analyzing the sample in the downstream position of the sample.
• the adjustment of the internal operating pressure is made using the breakdown detector, the adjustment comprises determining, for a given electric field, the operating pressure at the limit of the electrical breakdown.
• the method according to the invention makes it possible, for a given electric field, to find the operating pressure at the limit of electrical breakdown.
• FIG 1 illustrates an embodiment of the particle generator according to the invention with two possible positions of the sample and of the diagnostic module for the analysis of said sample.
• FIG. 1 illustrates an embodiment of the breakdown detector according to the invention.
• FIG. 1 illustrates an embodiment of the electrical circuit of the breakdown detector of the particle generator according to the invention.
• FIG 4 illustrates a first embodiment of the anode of the particle generator according to the invention.
• FIG 5 shows a second embodiment of the anode of the particle generator according to the invention.
• FIG 6 illustrates a sectional view of the anode, the section passing through the smaller diameter of the anisotropic anode.
• FIG. 7 illustrates different photo-triggering configurations of the charged particle generator according to the invention
• FIG 8 shows a method of calibrating the particle generator according to the invention.
• FIG. 1 illustrates an embodiment of the generator G of electrically charged particles according to the invention.
• the generator G will be referred to indifferently as the charged particle generator G or Mini Canon.
• the generator G is illuminated by a pulsed light source L emitting light pulses LP.
• the LP light pulses are sent to a T-tripler device to obtain LPJJV light pulses having a shorter wavelength than the LP pulses.
• the LPJJV beam is then sent to a PH photocathode.
• the LPJJV beam is focused using an LE lens so as to be focused on a specific point of the PH photocathode.
• the source is a pulsed source at 1064 nm and a frequency quadruple system is used to obtain light pulses with higher energy.
• the generator G further comprises means for modifying the point of arrival and the angle of attack of the LPJJV beam on the photocathode.
• the pulsed light source LP emits pulses having a central wavelength in the infrared.
• the pulses have a center wavelength of 800 nm with a repetition rate of 80 MHz.
• the temporal duration of the pulses is of the order of a few tens of fs.
• the light source L is a pulsed laser such as a femtosecond laser.
• the trigger laser is a pulsed UV, VIS or IR laser, or any other source of pulsed UV, VIS or IR light.
• the tripler T makes it possible to obtain LPJJV light pulses having a central wavelength approximately three times smaller than the wavelength of the pulses emitted by the source L.
• the light pulses coming from the tripler T have a central wavelength of the order of 266 nm.
• the light pulses of the LPJJV beam are suitable for generating photoelectrons at the level of the PH photocathode.
• the charged particle generator according to the invention further comprises a vacuum chamber V configured to maintain within it a working pressure of between 10 6 mbar, preferably 10 3 mbar, and atmospheric pressure.
• the vacuum chamber V comprises an optical window F allowing the passage of the LPJJV pulses intended to be focused on the photocathode PH.
• the vacuum chamber V has, in the axis of the charged particle beam, a window M transparent to said charged particles, the window M transparent to charged particles can for example be a membrane. This window M allows the charged particles to reach the sample E and the diagnostic module D 'when these are placed outside the vacuum chamber V.
• the window M has a thickness between 2 and 200 nm.
• the PH photocathode consists of a nanometric metallic stack on a thin optical strip type substrate, the nature of which is a function of the trigger wavelength and of the vacuum resistance. desired.
• the surface state of the constituent metal can be smooth or nanostructured.
• the substrate can be planar or shaped according to the desired spatial beam shaping.
• the generator G comprises an anode A positioned at a distance L from the photocathode PH and means for applying an electric field (or potential difference) between the photocathode and the anode.
• This electric field is also called the electron acceleration field.
• the distance L between photocathode PH and anode AN is adjustable and can be adapted to the chosen voltage.
• the distance L between the photocathode and the anode has a value of 300 ⁇ m for a polarization voltage of the photocathode in absolute value of 1 kV, or even 5 kV.
• this voltage in absolute value is of the order of 10, 20 or 30 kV
• this distance L is increased by a proportional factor of 10, 20 or 30 to avoid electrical breakdown, but the size of the device remains of the order of size of mm which is much less than the prior art.
• the module comprising the PH photocathode and the AN anode is machined, the electrodes not being movable.
• the change in the distance L between the electrodes is therefore done by substitution of the module comprising the electrodes, by choosing a module having a distance L adapted to the bias voltage of the chosen photocathode.
• the electrodes are mobile and the distance L is adjusted by moving the two electrodes apart or by bringing them together without changing the module.
• the distance L between photocathode PH and anode AN is less than 30 mm, preferably 10 mm.
• the invention makes it possible to reduce the distance L between photocathode PH and anode AN while using high operating pressures. This makes it possible to reduce the temporal dispersion of the electron packets generated and to obtain electron packets with a small temporal duration, for example less than or equal to 5 ps.
• the anode AN has an orifice or opening to allow the passage of the charged particles accelerated by the electric field applied between the photocathode PH and the anode AN.
• the anode AN has an orifice for passage of electrons having an anisotropic section in the plane normal to the electron beam.
• the anisotropic section of the orifice has two characteristic dimensions: a smaller diameter PD and a larger diameter GD, perpendicular to each other.
• Such an anode allows the use of the electron beam without passing through a downstream focusing lens which would be difficult to implement.
• the smaller diameter is significantly smaller than according to the embodiments of the prior art.
• the larger is greater than or equal to twice the smaller diameter.
• the small diameter is between 100 ⁇ m and 2 mm and the large diameter is between 100 ⁇ m and 20 mm.
• the anisotropic anode AN plays a role of filtering the electrons generated off-axis, so as to improve the emittance of the beam at the cost of the flow of electrons transmitted.
• this makes it possible to reduce the number of electrons and to limit the space charge effect which would reduce the temporal resolution of the Mini Canon.
• the anode does not appear as a ring or a pierced plate but as a juxtaposition in the same plane of two flat plates facing each other by two parallel lips so as to obtain an orifice for the passage of the charged particles in slot shape.
• This embodiment is illustrated in Figure 5.
• the generator G according to the invention further comprises a breakdown detector CL or spark gap.
• the detection of a breakdown ensures that, despite a low vacuum inside the Mini Canon, there will be no degradation of the components, in particular of the cathode and of the anode. There is no need for a real pressure measurement, but simply the assurance that at the working pressure chosen for the interior of the Mini Canon, there is no risk of breakdown.
• the use of a breakdown detector is counterintuitive for a person skilled in the art who would seek to use a means of measuring the pressure inside the vacuum chamber, while adjusting the pressure and tension to move away from it. more possible breakdown conditions.
• the breakdown detector CL or spark gap consists of a conductive ring placed opposite a point, the assembly being inserted just after the anode in the direction of propagation of the electrons.
• This spark gap is brought to the voltage at which one wishes to operate the enclosure of the Mini Canon, between 1 and 30 kV, preferably during an initial adjustment phase in a work campaign.
• the occurrence of a breakdown on the spark gap protects the functional elements, namely cathode and anode, separated by a distance L slightly greater than the distance between the elements of the spark gap.
• the breakdown detector CL allows, for a chosen working voltage, to come very close to the breakdown without exposing the functional components in operation mode.
• the charged particle generator according to the invention provides packets of charged particles having a very short time duration, while working with a high pressure inside the enclosure. empty.
• the breakdown detector it is possible to analyze fragile samples, liquid or biological, with a temporal resolution of the order of the picosecond.
• the sample to be analyzed E can be placed both inside or outside the vacuum chamber V.
• a diagnostic module for analyzing the sample D ' is always placed downstream of the sample to be analyzed E. It can be seen in figure 1 that when the sample E is placed inside the vacuum chamber V, the diagnostic module D' can be placed at inside or outside said enclosure V. When the sample to be analyzed E is outside, the diagnostic module D 'is also outside.
• the diagnostic module D ′ is placed at a distance d2 from the sample E such that 0 ⁇ d2 ⁇ 60mm. It is important that the sample to be analyzed is not in contact with the diagnostic module in order to avoid a transfer of charges.
• the distance d between the photoemissive cathode and the sample is between 1 mm for a bias voltage of the photocathode less in absolute value than 1 kV, and 30 mm for a bias voltage of the photocathode of the order of 30 kV in absolute value.
• a small distance between the anode AN and sample to be analyzed E makes it possible to limit the temporal dispersion of the electron packets and to obtain a high temporal resolution. So when the sample E is inside the enclosure V, the sample E to be analyzed is at a distance d1 such that 0 ⁇ d1 ⁇ 0.7 mm.
• the generator G can comprise another diagnostic module D, placed as close as possible to the anode, for determining the temporal duration of the packets of electrons or of particles. charged, it is used to calibrate the generator according to the laser used, and then it is removed during sample measurements.
• This further diagnostic module D can be used with an anisotropic anode having a slit-shaped opening.
• the electrically charged particles are gas ions.
• the following elements are added downstream of the electron beam to obtain a gas ion generator: a gas capable of emitting positive ions during electron bombardment; at least one ion beam focusing anode.
• FIG. 2 illustrates an embodiment of a breakdown detector or spark gap CL according to the invention.
• a value of 1.5 kV.mrrr 1 corresponds to the vacuum breakdown threshold at 10 4 mbar, a value of 3 kV.mnr 1 corresponds to the vacuum breakdown threshold at 10 5 mbar.
• the Mini Canon approaches very close to the breakdown condition: the device according to the invention works at the limit of breakdown, on the one hand because it is necessary to bring high voltages to reduced dimensions, on the other hand because the insertion of a sufficiently miniaturized pressure gauge for the system is not possible.
• a breakdown detector CL comprising a spark gap set to a voltage slightly lower than the breakdown voltage of the barrel, and giving a warning signal allowing the operating conditions to be somewhat deviated from the breakdown conditions.
• the breakdown detector CL comprises: a substrate 1 made of insulating material with a high dielectric constant, for example of Peek; an electrically conductive ring 2 connected to an equally conductive rod 3, the two being electrically connected and brought to the potential of the anode; a conductive rod 4 sliding in its bore, able to move radially, for example under the effect of a micrometric screw, not shown.
• the end of the rod 4 which can hardly be seen protruding in the central bore, is placed at a distance slightly less than the distance of the shortest electrical path between anode AN and photocathode PH.
• this distance AN anode and photocathode PH varies according to the voltage at which one chooses to make the enclosure of the barrel work, the distance between the end of the rod 4 and the ring at the potential of the anode must be adjusted accordingly , so as to have the same value or to be very slightly below.
• the rod 4 is integral with the cathode PH, so that when the distance between anode AN and photocathode PH is adjusted, the distance between the apex of the rod is modified at the same time and in the same proportions. 4 and ring 2.
• the anode AN and the photocathode PH are separated by a distance L of 300 ⁇ m.
• the electrical resistance of air at atmospheric pressure is 36 kV cm 1 which is equivalent to 300 ⁇ m for a potential difference of 1080 V.
• the device according to the invention can operate up to 10 kV, this is not possible. sufficient to avoid breakdown, thus creating a vacuum allows increase this maximum voltage before creating an electric arc which could damage the system and create a risk for the user.
• the device according to the invention does not require any heavy and constantly active device such as devices working under a vacuum greater than 10 5 mbar, and often greater than 10 7 mbar.
• the exact measurement of the pressure is not necessary for the use of the device according to the invention.
• the device according to the invention makes it possible to alert the user or to stop the system when the pressure is no longer low enough and this may represent a risk of breakdown
• the system comprises a mass connected to an electronic card. This mass is placed so that it is closer to the anode than the cathode, thanks to a calibrated ring which serves as an insulating spacer. The breakdown between the anode and the earth will therefore occur earlier and we can thus process the information upstream of the breakdown of the system.
• the breakdown detection circuit illustrated in FIG. 3, receives the voltage of the photocathode PH in "Vin", while the rest of the circuit and the anode AN are referenced to ground. With each spark, a pulse is generated on the “Vout” output. The signal at the "Vout” output can therefore be used to alert the user to the risk of electrical breakdown.
• FIGS. 4 and 5 discussed above, illustrate the two embodiments of the AN anode having an anisotropic opening.
• Figure 6 illustrates a sectional view of the anode AN, the section passing through the smallest diameter of the anode AN.
• the anode is deposited on an insulating sapphire substrate S 700 ⁇ m thick, orthogonal to the axis z corresponding to the axis of propagation of the electron beam.
• the anode AN is one and the same electrode consisting for example of a conductive film affixed to a perforated substrate.
• the passage opening for the charged particles can be slit-shaped, as illustrated in FIG. 5.
• the large diameter GD extends to the ends of the anode so as to cut it into two distinct elements mechanically linked together by an insulating element.
• the anode AN then comprises two parallel lips, one subjected to a voltage U - Dn, and the other to U + Dn.
• such a slot-shaped anode may consist of a conductor affixed to a substrate S, the assembly having been cut by an elongated slot along y of very small dimensions along x, to parallel edges.
• this configuration it is possible to obtain two separate electrodes brought to a potential of one or more kV with respect to the emissive cathode, but electrically isolated from each other. They can thus have between them a low potential difference compared to the voltage of the cathode, but which can be of a few tens or hundreds of volts, thus creating an electric field E between their lips.
• This electric field E can vary over time in synchronism with the arrival of the electron packets, so that the two ends of the electron packet do not see the same field E.
• the first electron of each bunch sees a strong field E which deflects it towards the electrode E2, and this field decreases for the following electrons until a zero field for the last of the bunch.
• This has the effect of rotating the axis of the electron bundle, and thus increasing its projection perpendicular to the axis of propagation, and allowing a spatial measurement from which we will deduce a temporal measurement.
• the electrodes E1 and E2 constitute a microstrip line "coplanar microstrip line" with an impedance of 50 W which allows extremely rapid rising or falling edges along these electrodes.
• the anode when the anode consists of two facing flat lips, these two lips spaced apart by a small and strictly constant distance are brought to different potentials. This is advantageous when the generator G is pulsed with pulses of short duration ps or fs resulting in small packets of electrons. The anode then performs several functions simultaneously.
• the constant potentials VE1 and VE2 applied to the electrodes E1 and E2 have a relatively small difference AVE but which varies over time.
• the anode then has, in addition to its accelerating function, that of a deflector which allows a temporal diagnosis of the electron beam.
• this embodiment allows the integration of a scanning system directly at the anode.
• Example of an anode with an integrated scanning system the electrodes are designed to form a 50 W line in "coplanar microstrip line". This configuration will test the time resolved scan mode of this device.
• the anode plate is the most complex part of the device. It is a 700 ⁇ m sapphire substrate cut so as to leave the electrodes out and split in the middle to allow the electrons to pass, for example with a slit of 100 ⁇ m. The rear face is possibly thinned in the middle to avoid any contact with the sample plate.
• the beam In static mode, without differential voltage on the electrodes of the anode, the beam maintains a reduced dimension of less than 20 ⁇ m.
• the dimension of the electron beam is greater than the dimension of the photon beam incident on the photocathode, but of the same order of magnitude.
• this size In scanning mode, with voltages on the anode electrodes, this size is kept with a sensitivity of the order of of 100 miti / 100V or a simulated displacement of 200 miti at the sample level for voltages +/- 100 V for the electrodes.
• the maximum deflection depends on the geometry of the slot and is of the order of 1 mm for voltages of +/- 500 V. These values are valid for a displacement perpendicular to the slot and measured at 700 miti from the anode, at the sample level.
• the distance d1 between the anode AN and the sample E to be analyzed is small and less than 60 mm, preferably 0 ⁇ d1 ⁇ 0.7 mm. Accordingly, it may be advantageous to place sample E inside or outside the charged particle generator G. It is important that the sample to be analyzed is not in contact with the anode in order to avoid charge transfer, except in the case where the potential of the anode and of the sample are zero.
• Mini Canon in a horizontal or vertical position on an optical bench or on any other assembly, given that the incidence of the triggering laser beam can be perfectly controlled. Liquid samples can then be analyzed with a beam in a vertical position.
• a drop of the sample is positioned on an output interface adapted to the energy of the electrons, for example an ultrathin membrane of S13N4 or graphene having a thickness between 2 nm and 200 nm.
• the electron beam is directed at a sample placed in a vacuum chamber.
• the device according to the invention offers the possibility for the sample to remain at atmospheric pressure, since the electron beam is exited from the mini cannon which constitutes a miniaturized vacuum chamber.
• a variant for the study of samples supporting the vacuum consists in placing the sample directly in the enclosure of the Mini Canon, as close as possible to the emission, the detection of the phenomenon to be studied, for example scintillation, can be performed by a detector directly behind the sample.
• the sample can be designed as a module of the Mini Canon, just like the photocathode, anode or detector.
• FIG. 7 illustrates different geometric configurations for the photo-triggering of the device.
• One of the ways of proceeding is to send the LPJJV laser at an incidence different from the normal incidence on the PH photocathode, so that the laser beam and the electron beam are not collinear on the target.
• the slit of the anode AN is sufficiently closed so that the LPJJV beam does not pass through the system.
• an angle of 30 to 45 ° can be used on this geometry.
• the firing axis of the laser impacts the target at a point and at an adjustable angle.
• the angle of impact is different from 90 °, and preferably between 30 and 45 °.
• these embodiments make it possible to increase the precision and reliability of the analyzes thanks to a better separation of the electron beam and the LPJJV beam at the level of the sample and of the detection module used for the analysis. .
• the point of impact on the photocathode is placed at an eccentric point, and the photocathode is rotated manually without dismantling (and without modifying the pressure in the enclosure) when one wishes to modify the point impact.
• the modification of the point of impact of the laser can be done either by moving the photocathode in its cradle or by modifying the direction of the laser on the slit.
• the modification of the point of impact of the laser on the photocathode is done without breaking the vacuum inside the enclosure V.
• a mini ion pump can be connected to the mini enclosure depending on the duration of the desired experiment (up to 1 week in static vacuum is currently possible)
• the sample to be studied must be placed in the enclosure of larger dimension before it is evacuated, the coupling valve is located on the side of the output module, The vacuum is managed by the system of reception which can be from 10 5 to 10 7 mbar, or even below.
• the detection means are coupled to the existing system itself.
• the third is made at atmospheric pressure with an autonomous system and was carried out as follows:
• a mini ionic pump can be connected to the mini enclosure depending on the duration of the desired experiment (up to 1 week in static vacuum is currently possible). In this configuration, the voltage is from -10 kV and above to allow air extraction through the membrane.
• the sample to be studied remains outside the mini enclosure and will be placed on the ultrathin outlet membrane placed horizontally, or vertically if it is a vertical liquid or gas jet.
• the fourth is made at atmospheric pressure with an autonomous system and was carried out as follows:
• the voltage is from -10 kV and beyond in order to allow the extraction with air through the membrane, the sample to be studied remains outside the mini enclosure and will be placed on the ultrafine membrane at the outlet placed horizontally, or vertically if it is a vertical liquid or gaseous jet.
• the vacuum is generally managed by the reception system which can be from 10 5 to 10 7 mbar, or even below.
• the detection means are coupled to the reception system itself.

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• 2019
  • 2019-07-02 FR FR1907324A patent/FR3098341A1/fr active Pending
• 2020
  • 2020-06-30 WO PCT/EP2020/068427 patent/WO2021001383A1/fr unknown
  • 2020-06-30 US US17/623,941 patent/US20220367139A1/en active Pending
  • 2020-06-30 EP EP20734958.0A patent/EP3994714A1/de active Pending
  • 2020-06-30 JP JP2021578031A patent/JP2022539216A/ja active Pending
  • 2020-06-30 CA CA3145386A patent/CA3145386A1/fr active Pending

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