WO2015053300A1 - Microscope électronique - Google Patents

Microscope électronique Download PDF

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Publication number
WO2015053300A1
WO2015053300A1 PCT/JP2014/076883 JP2014076883W WO2015053300A1 WO 2015053300 A1 WO2015053300 A1 WO 2015053300A1 JP 2014076883 W JP2014076883 W JP 2014076883W WO 2015053300 A1 WO2015053300 A1 WO 2015053300A1
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WO
WIPO (PCT)
Prior art keywords
electron
electron source
current
emission
flushing
Prior art date
Application number
PCT/JP2014/076883
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English (en)
Japanese (ja)
Inventor
大西　崇
渡辺　俊一
Original Assignee
株式会社日立ハイテクノロジーズ
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 株式会社日立ハイテクノロジーズ filed Critical 株式会社日立ハイテクノロジーズ
Priority to JP2015541606A priority Critical patent/JP6129982B2/ja
Publication of WO2015053300A1 publication Critical patent/WO2015053300A1/fr

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    • 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
    • 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
    • H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
    • H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
    • 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
    • H01J2237/245—Detection characterised by the variable being measured
    • H01J2237/24507—Intensity, dose or other characteristics of particle beams or electromagnetic radiation
    • H01J2237/24514—Beam diagnostics including control of the parameter or property diagnosed
    • H01J2237/24535—Beam current

Definitions

  • the present invention relates to an electron microscope.
  • the present invention relates to a cold cathode field emission (Cold-FE) electron gun that generates a particularly bright electron beam and an electron microscope equipped with the Cold-FE electron gun.
  • Cold-FE cold cathode field emission
  • An electron microscope is an observation device that uses an electron beam to obtain an enlarged image of a sample and information on constituent elements.
  • the electron microscope mainly includes an electron gun, an electron optical system, a sample holder, a detector, a control device, and a power supply unit.
  • An electron gun is a device that generates an electron beam.
  • the electron optical system is a device that transports electrons generated by an electron gun and irradiates a sample.
  • the electron optical system also has a function of converging and deflecting an electron beam by an electromagnetic lens.
  • the sample holder is a device that fixes a substance to be observed (that is, a sample) on the electron beam path in the electron optical system, and moves and tilts it as necessary.
  • the electron gun and the electron optical system are maintained in a vacuum in order to pass an electron beam without colliding with air molecules, and are equipped with a vacuum exhaust device for that purpose.
  • Electrons irradiated on the sample generate reflected electrons, secondary electrons, transmitted electrons, scattered electrons, X-rays, and the like due to the interaction with atoms constituting the sample.
  • the detector measures these electrons and X-rays.
  • the power supply unit supplies power necessary for the operation of the electron gun, the electron optical system, the detector, and the like, and performs precise control.
  • the control device controls the power supply, analyzes information obtained by the detector, and processes, displays, or records an enlarged image of the sample and the elemental composition of the sample in an easy-to-see state for the operator.
  • An electron gun generates electrons used for observation as free electrons in a vacuum based on various principles. Furthermore, the generated free electrons are accelerated by the potential difference potential to form a group of electrons having kinetic energy, that is, an electron beam.
  • the electron dose per unit time generated by the electron source in the electron gun is called the emission current. Further, a part of this emission current is taken out through the diaphragm, and irradiated onto the sample to generate probe electrons for obtaining an enlarged image or the like.
  • the probe electron dose per unit time is called a probe current.
  • Cold-FE electron gun which is a kind of electron gun
  • Cold-FE electron guns use tungsten single crystals with sharp tips sharpened by electropolishing as electron sources.
  • An extraction voltage of several kilovolts is applied between the extraction electrode adjacent to the electron source and the electron source. Electric field concentration occurs at the tip of the electron source. Due to this high electric field, electrons due to field emission are emitted from the tip of the electron source.
  • the amount of electron beam emitted is the emission current described above. In the Cold-FE electron source, the emission current is emitted from the electron source within a solid angle range of about 1 steradian.
  • the emission current is influenced by the surface condition of the electron source as well as the extraction voltage (or the electric field strength at the tip of the electron source).
  • the Cold-FE electron source is a tungsten single crystal placed in an electron gun whose residual gas pressure is lowered by a vacuum pump.
  • the work function of the electron source generally decreases. Therefore, the amount of electron beam emission decreases as the residual gas molecules collide with the electron source and are adsorbed.
  • the emission current gradually decreases under a constant extraction voltage.
  • a process for cleaning the surface of the electron source by, for example, re-releasing the adsorbed gas molecules into a vacuum is required. This is achieved by instantaneously heating the single crystal. Therefore, many Cold-FE electron guns are cleaned by heating the electron source by welding the electron source to the filament tip and heating the filament for a short time. This is called flushing. When flushing is performed, the tip of the electron source is cleaned. In the Cold-FE electron gun, this flushing is performed periodically to obtain a constant emission current. The required flushing frequency varies with the residual gas pressure in the electron gun.
  • the Cold-FE electron gun requires flushing of the electron source.
  • the electron source flushing maintains the cleanness of the tip of the electron source, and a stable emission current can be obtained.
  • the flushing causes movement (drift) of the tungsten atoms at the tip of the electron source due to heat, so that the physical shape of the tip gradually changes each time flushing is repeated. This change is usually due to the attractive force acting between the atoms in the crystal, causing the physical shape of the sharply pointed tip to gradually round (this is the “rounding” of the electron source tip. Called).
  • the radius of curvature of the electron source tip gradually increases, and as a result, the electric field concentration at the electron source tip is weakened.
  • the extraction voltage for obtaining the same emission current or probe current increases.
  • the extraction voltage gradually increases over the usage period of the electron gun. If this extraction voltage exceeds the limit voltage of the electron gun (determined by the power supply capability and the insulation performance within the wiring and the electron gun), sufficient probe current cannot be obtained from this electron source, and the electron source must be replaced. Necessary.
  • the strength of flushing can be adjusted as the amount of current flowing through the filament.
  • the electron source By passing more current, or for a relatively long period of time, the electron source becomes hotter “strong flushing”. At this time, the tip of the electron source is further cleaned, but the degree of rounding is large.
  • the temperature at the tip of the electron source becomes relatively low, resulting in “weak flushing” with less rounding per flushing.
  • the tip is not sufficiently cleaned. In such a case, the extraction voltage required for extracting the same emission current becomes high, or the field emission becomes unstable and the probe current largely fluctuates in a short time. An observation image cannot be obtained.
  • the required flashing strength is defined as the filament current
  • the flushing with sufficient strength is performed in advance at a frequency that is considered sufficient in advance, so that both the cleaning of the electron source and the lifetime of the electron source are achieved. I was planning.
  • the flushing period during the operation of the electron gun is performed by the user judging whether the probe current is not reduced or unstable, or whether a good observation image is obtained.
  • the problem to be solved is that an electron microscope user or an electron microscope control device obtains an appropriate flashing timing and flashing strength in an electron microscope equipped with a Cold-FE electron gun.
  • the present invention adopts the configuration described in the claims to solve the problem.
  • the emission current which is the total current obtained by field emission from the electron source, is measured, and the measured value is used to indicate the appropriate flashing time and intensity to the user, or automatically Implement appropriate flushing.
  • the Cold-FE electron gun of the present invention can obtain a more stable probe current without replacing the electron source for a longer period of time by performing flushing with an appropriate intensity at an appropriate time. As a result, it is possible to obtain an electron microscope that does not require maintenance for a long time and can obtain a higher quality observation image.
  • the measurement results of the temporal change in the emission current emitted from a clean electron source or an electron source with gas molecules attached are shown, and in the embodiment of the invention, which is used to distinguish between a clean electron source and an electron source with gas molecules attached It is a measurement result and explanatory drawing explaining how to carry out.
  • the Example of invention it is the figure which illustrated the display which notified the time of strong flushing and the strong flushing to the user automatically from the temporal change of emission current, and the cleanliness of the electron source.
  • FIG. 1 shows an electron microscope equipped with a Cold-FE electron gun as an example of an embodiment for carrying out the invention.
  • the electron microscope includes an electron gun 1, an electron optical system 2, a sample holder 3, a detector 4, a control device 5, and a power supply unit 6.
  • the electron gun 1 and the electron optical system 2 have vacuum evacuation devices 11 and 21, respectively. However, depending on the scale of the electron microscope, there may be a single vacuum evacuation device. In some cases, a large number of vacuum evacuation devices are provided.
  • the electron gun 1 including the Cold-FE electron source 101 generates an electron beam 10.
  • the electron optical system 2 converges and deflects the electron beam 10 and irradiates the sample 31.
  • the sample holder 3 holds the sample 31 and moves, tilts and exchanges as necessary.
  • the detector 4 measures reflected electrons, secondary electrons, transmitted electrons, scattered electrons, X-rays, etc. generated by the sample 31.
  • the power supply unit 6 supplies power to the electron gun 1 and the electron optical system 2, adjusts the output, and controls the electron beam to a state requested by the operator. Moreover, the information from the detector 4 is converted into a digital signal.
  • the control device 5 controls the electron gun 1 and the electron optical system 2 through the power supply system 6, processes information from the detector 4, and displays or records the information in a form visible to the operator.
  • the power supply system 6 is divided into a control / detection system power supply 61 and an electron gun power supply 62.
  • FIG. 2 shows details of the structure of the Cold-FE electron gun 1 having an acceleration voltage of several hundred kilovolts, which is an embodiment of the present invention.
  • the electron gun 1 includes an electron source 101 (cold cathode field emission electron source), an extraction electrode 103, and an acceleration tube 105.
  • the electron gun 1 is connected to an electron gun power source 62 and is given a high potential.
  • An extraction voltage (V 1 ) of several kilovolts is applied to the extraction electrode 103 by an extraction power source 621.
  • V 1 an extraction voltage
  • the acceleration tube 105 includes a plurality of intermediate electrodes 104, 106, 107, 108, and 109, and the electron beam is further accelerated while passing through the intermediate electrodes.
  • the electron source 101 and the extraction electrode 103 are under a negative high voltage (V 0 ) of several hundred kilovolts by the acceleration power source 623.
  • the anode 110 is at ground potential and is at zero potential. The electron beam is accelerated by this potential difference, and the electrons passing through the anode 110 are electron beams having V 0 energy.
  • the extraction power source 621 has a function of stably applying an extraction voltage to the extraction electrode 103 and a function of measuring a current flowing through the power source.
  • An ammeter 63 is shown in the figure.
  • the extraction electrode is insulated from other electrodes by an insulator, and apart from a minute discharge current, all of the flowing current is due to an emission current due to field emission from the electron source. Therefore, if the current flowing between the extraction electrode and the electron source with the extraction power source is measured by the ammeter 63, this is approximately equal to the emission current. This value is Ie.
  • the extraction power source and the electron gun power source send this current amount Ie as measurement data to the control device 5 shown in FIG. 1 as a digital signal.
  • the control device 5 records this emission current data.
  • the flushing power source 624 is a power source that controls the current flowing through the filament 102 to which the electron source is fixed.
  • the flushing power source 624 supplies current to the filament 102 to which the electron source is fixed.
  • the filament 102 is heated by this Joule heat, the temperature of the electron source 101 rises, and the surface of the electron source 101 is cleaned.
  • the flushing intensity at this time is controlled by the magnitude of the current flowing through the filament, for example, by the control device controlling the flushing power source 624.
  • FIG. 3 shows a typical example of the temporal change in the emission current emitted from the electron source after the flushing and the probe current that has passed through the diaphragm 121.
  • the emission current decreases relatively monotonously, but the probe current maintains (1) a value close to a high constant value for a certain period of time. Thereafter, (2) after a rapid decrease, (3) shift to a low constant value.
  • the emission current is physically an electron beam emitted from a relatively wide area of the electron source surface, whereas the probe current is near the tip of the electron source. And an electron beam emitted from a relatively narrow area emitted from the electron beam. For this reason, the field emission (emission current) from the tip of the electron source consisting of a large number of atoms decreases stably, whereas the probe current shows a relatively unstable behavior, and the increase / decrease stepwise. It may be seen.
  • the region on the electron source involved in the generation of the probe current is narrow, and only a relatively small number of atoms on a specific crystal plane contribute to the emission, so the probe current varies widely due to the stochastic effect of residual gas molecules. It is thought that it is to do.
  • the probe current starts to decrease sharply.
  • the amount of current also fluctuates unstable. This can be determined by measuring the probe current.
  • the timing ( ⁇ 50 ) at which the emission current is reduced to 50% of the emission current Ie 0 immediately after the flushing shown in the figure corresponds to the time when the probe current is almost 80%. Confirmed to do.
  • the electron source can be utilized most effectively if the emission current is measured and flushing is performed at the timing ( ⁇ 50 ) when Ie is reduced to 0.5Ie 0 .
  • the dialog box or the like to recommend flushing when reduced to 50% of the flushing after emission current Ie 0, prompting the flushing user.
  • flushing is performed at the timing when the user removes the seat or replaces the sample to clean the electron source.
  • a display example to the user is shown in FIG.
  • a dialog such as 91 is displayed on the screen of the control device 5 being viewed by the user to prompt the user to flush.
  • the user instructs the control device 5 to perform flushing by a button on the dialog or other method, and cleans the electron source.
  • the control device 5 senses the information and automatically performs flushing. In this case, it is desirable to notify the user by issuing a dialog such as 92 that the flushing has been performed.
  • the elapsed time from the last flushing, the next flushing time, and the current emission current which is a measure of the time until the next flushing, are displayed on the control device 5 in a manner like 93 to alert the user. can do.
  • the last flushing time, the next flushing time expected from the emission current value, and the current emission current Ie value are compared with the initial emission current Ie 0 and displayed in the form of a band graph. .
  • the control device can know the appropriate time for flushing, and can notify the user in an easy-to-understand manner. In response to this information, the control device can prompt the user to perform flushing or automatically perform flushing to keep the electron source in a good state.
  • flushing is performed for cleaning the surface of the electron source. How much flushing is required for cleaning the surface of the electron source depends on the surface condition of the electron source. Depends on. An electron source to which a larger amount of gas molecules is adsorbed needs to be cleaned by strong flushing, but can be cleaned by weak flushing if the amount of attached gas molecules is small. Gas molecule adsorption is thought to depend on the type of residual gas molecules adsorbed on the electron source, and qualitatively lighter atoms (such as hydrogen atoms) are removed from the electron source at a relatively low temperature, but heavy. When molecules (such as hydrocarbons) are adsorbed, strong flushing is required.
  • the temporal change of the probe current will not be standard as shown in the lower part of FIG.
  • the stable region (1) becomes shorter, the unstable region (2) arrives earlier, or the stable region (1) does not appear and a constant value region (3) with low luminance appears immediately after flushing.
  • FIG. 5 shows an example of temporal changes in the emission current corresponding to the state where these electron sources are clean and the state where many gas molecules remain.
  • the time variation of the emission current is recorded in a clean electron source state, it stabilizes at about 1/10 (0.1 Ie 0 ) of the initial emission current after a certain time.
  • the emission current in the stable period becomes a large value such as 1/5 or 1/3 of the initial value, and does not decrease any further.
  • the emission current after a long period of time has elapsed compared to Ie 0 does not converge to 0.1Ie 0, it becomes a larger value than that of the Ie 0.
  • Whether the electron source is cleaned may be determined by measuring the convergence value of the emission current after long-term observation.
  • the time shown on the horizontal axis is normalized with the time ( ⁇ 50 ) when the emission current becomes 0.5 Ie 0 being 1.
  • the group (A) where the electron source is cleaned is convex upward at 0.5 ⁇ 50 .
  • the curve representing the temporal change of the emission current is convex downward in the group (B) at this time.
  • the group (C) indicating an intermediate cleanliness is intermediate between (A) and (B).
  • the control device 5 records the temporal change of the emission current measured as the output from the electron gun power supply 62, and particularly the time ⁇ 50 when the emission current Ie becomes 0.5Ie 0.
  • the emission current Ie 0.5 at time 0.5 ⁇ 50 is extracted.
  • Ie 0.5 and Ie 0 are compared, and if the value is, for example, 75% or more, it is determined that the electron source is clean.
  • Ie 0.5 is less than this value, it is judged that many gas molecules remain in the electron source, and it is recommended that the flashing intensity is automatically increased or the user is notified to perform strong flushing.
  • a display example to the user is shown in FIG.
  • a dialog such as 94 is displayed on the screen of the control device 5 viewed by the user, prompting the user to perform strong flushing.
  • the user instructs the control device 5 to perform flushing by a button on the dialog or other method, and cleans the electron source by intensely heating it.
  • the control device 5 senses the information and automatically performs strong flushing. In this case, it is desirable to notify the user that a strong flushing has been performed by issuing a dialog such as 95.
  • the time when Ie 0.5 was last measured and the value of Ie 0.5 which is a measure of the degree of cleanliness of the electron source, can be displayed on the control device 5 by a method such as 96 to alert the user.
  • a method such as 96 to alert the user.
  • the time when Ie 0.5 was last measured and the cleanliness of the chip that can be distinguished from Ie 0.5 are displayed in the form of a band graph. If there are many gas molecules attached to the chip, the user can perform strong flushing and determine the effect by this band graph.
  • Electron gun evacuation apparatus 101
  • Electron source 102
  • Filament 103
  • Extraction electrode 104
  • Adjustment electrode 105
  • Accelerating tube 106
  • Intermediate electrode 107
  • Intermediate electrode 109
  • Anode 17
  • Ion pump 2
  • Electron optical system 21
  • Electron optical System vacuum evacuation device 3
  • Sample holder 31
  • Control device 6
  • Power supply 61
  • Example of dialog prompting user to flush 92
  • Example of dialog notifying the user of flushing 93
  • Example of display notifying the user of flushing time 94
  • Example of dialog prompting the user to perform strong flushing 95 Display example to notify the cleanliness of the electron source in Example 96 user of the dialog to notify the

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Electron Sources, Ion Sources (AREA)

Abstract

　La présente invention a pour objet de mesurer le courant d'émission dans un microscope électronique équipé d'un canon à électrons de type à émission de champ à cathode froide (1), pour obtenir le facteur de propreté de la source d'électrons (101). En prenant l'instant auquel le courant d'émission atteint 0,5 juste après le flashage comme occasion de nettoyer la source d'électrons (101), le changement temporel du courant d'émission consécutif au flashage sert à estimer le facteur de propreté de la source d'électrons (101), et un flashage plus intense est effectué.
PCT/JP2014/076883 2013-10-10 2014-10-08 Microscope électronique WO2015053300A1 (fr)

Priority Applications (1)

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JP2015541606A JP6129982B2 (ja) 2013-10-10 2014-10-08 電子顕微鏡

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JP2013212424 2013-10-10
JP2013-212424 2013-10-10

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WO2015053300A1 true WO2015053300A1 (fr) 2015-04-16

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019155540A1 (fr) * 2018-02-07 2019-08-15 株式会社日立ハイテクノロジーズ Dispositif de nettoyage
US11398364B2 (en) * 2019-10-07 2022-07-26 Jeol Ltd. Electron gun, electron microscope, three-dimensional additive manufacturing apparatus, and method of adjusting current of electron gun

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JPH0487244A (ja) * 1990-07-27 1992-03-19 Hitachi Ltd 走査型電子顕微鏡
JPH0525654U (ja) * 1991-09-17 1993-04-02 株式会社日立製作所 走査電子顕微鏡
JPH0845455A (ja) * 1994-07-27 1996-02-16 Jeol Ltd 電界放射型電子銃の動作状態判断方法
JPH08129981A (ja) * 1994-10-28 1996-05-21 Hitachi Ltd 電界放射型電子銃及び電子線装置
JP2005235469A (ja) * 2004-02-18 2005-09-02 Jeol Ltd 荷電粒子ビーム装置及び荷電粒子ビーム装置の制御方法
JP2011171088A (ja) * 2010-02-18 2011-09-01 Hitachi High-Technologies Corp 電界放出電子銃及びその制御方法

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0487244A (ja) * 1990-07-27 1992-03-19 Hitachi Ltd 走査型電子顕微鏡
JPH0525654U (ja) * 1991-09-17 1993-04-02 株式会社日立製作所 走査電子顕微鏡
JPH0845455A (ja) * 1994-07-27 1996-02-16 Jeol Ltd 電界放射型電子銃の動作状態判断方法
JPH08129981A (ja) * 1994-10-28 1996-05-21 Hitachi Ltd 電界放射型電子銃及び電子線装置
JP2005235469A (ja) * 2004-02-18 2005-09-02 Jeol Ltd 荷電粒子ビーム装置及び荷電粒子ビーム装置の制御方法
JP2011171088A (ja) * 2010-02-18 2011-09-01 Hitachi High-Technologies Corp 電界放出電子銃及びその制御方法

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2019155540A1 (fr) * 2018-02-07 2019-08-15 株式会社日立ハイテクノロジーズ Dispositif de nettoyage
CN111727488A (zh) * 2018-02-07 2020-09-29 株式会社日立高新技术 清洁装置
JPWO2019155540A1 (ja) * 2018-02-07 2021-01-28 株式会社日立ハイテク クリーニング装置
US11244806B2 (en) 2018-02-07 2022-02-08 Hitachi High-Tech Corporation Cleaning device
JP7132254B2 (ja) 2018-02-07 2022-09-06 株式会社日立ハイテク クリーニング装置
CN111727488B (zh) * 2018-02-07 2023-06-06 株式会社日立高新技术 清洁装置
US11398364B2 (en) * 2019-10-07 2022-07-26 Jeol Ltd. Electron gun, electron microscope, three-dimensional additive manufacturing apparatus, and method of adjusting current of electron gun

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