WO2010070837A1 - 電子線装置およびそれを用いた電子線応用装置 - Google Patents
電子線装置およびそれを用いた電子線応用装置 Download PDFInfo
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- WO2010070837A1 WO2010070837A1 PCT/JP2009/006637 JP2009006637W WO2010070837A1 WO 2010070837 A1 WO2010070837 A1 WO 2010070837A1 JP 2009006637 W JP2009006637 W JP 2009006637W WO 2010070837 A1 WO2010070837 A1 WO 2010070837A1
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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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/28—Electron or ion microscopes; Electron or ion diffraction tubes with scanning beams
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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
- H01J37/065—Construction of guns or parts thereof
-
- 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
- H01J37/075—Electron guns using thermionic emission from cathodes heated by particle bombardment or by irradiation, e.g. by laser
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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
- H01J37/252—Tubes for spot-analysing by electron or ion beams; Microanalysers
- H01J37/256—Tubes for spot-analysing by electron or ion beams; Microanalysers using scanning beams
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- 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
- H01J2237/06308—Thermionic sources
- H01J2237/06316—Schottky emission
Definitions
- the present invention relates to an electron beam apparatus equipped with functions such as low acceleration, high resolution, high current, and high-speed elemental analysis, and an electron beam application apparatus using the same, and in particular, observes a microstructure using an electron beam.
- the present invention relates to a scanning electron microscope (SEM).
- SE electron source A key emission electron source (hereinafter referred to as SE electron source) is used.
- SE electron source the tip of a W (100) single crystal rod with a thickness of about 0.1 mm is sharply pointed, Zr and O are adsorbed on this surface, and only the (100) plane is selectively set to a work function of about 2.8 eV.
- the W single crystal rod is fixed on a heating element made of a W filament and heated to a temperature of about 1800K for use.
- a large radius of curvature r is preferable. This is disclosed in Patent Document 1, for example. In this case, it has been considered preferable that r is 1 ⁇ m or more and 2 ⁇ m or less.
- a surface structure having a work function lower than that of Zr-O / W and operating at a low temperature is required.
- the Zr-O / W system has a work function of 2.8 eV and an operating temperature of around 1800 K, while the Ba-O / W system has a work function of 1.0-1.5 eV and an operating temperature of about 1000-1200 K, with an energy range of Is described in Non-Patent Document 1 (FIG. 4, section 6.2 on the right side of p.441, from the beginning to the fourth line).
- Patent Literature 3 describes various element and compound candidates.
- JP-A-2005-339922 JP 09-283068 A Japanese Patent Laid-Open No. 11-224629
- the radius of curvature r of the tip is larger than 0.5 ⁇ m and smaller than 1 ⁇ m.
- a conical cone angle ⁇ at a position 3r to 8r from the tip is larger than 5 ° and smaller than 8 / r °.
- the unit of r is ⁇ m.
- Ba is used instead of Zr, and this Ba diffusion supply means is composed of a porous metal sintered body and a Ba diffusion source containing Ba—O.
- the main point of the present invention is an SE electron source composed of a metal sintered body useful for observing a SEM image with low acceleration and high resolution and a Ba diffusion source containing Ba oxide.
- FIG. 1 shows an example of an electron beam application apparatus according to the present invention.
- Fig.1 (a) has a W needle 1 as an electron emission source, a heating element 3 by a W filament that supports it, and a diffusion source 2 of Zr-O, which are held on an insulator 5 and an electrode 4 to generate thermoelectrons.
- Suppressor 6 is placed on the needle, and the needle-like tip 8 of the W needle (single crystal W metal needle) 1 gradually becomes thinner from the cylindrical shape of the W single crystal rod as shown in FIG.
- this portion is a connected portion (here, this portion will be referred to as a “necked portion” for convenience), and this length Ln is preferably 200 ⁇ m or less so as to keep the strength of the needle and to make the diffusion distance moderately short.
- the radius of the sphere when the tip is approximated to a hemispherical shape is called a radius of curvature r of the tip, and this r is 0.5 ⁇ m ⁇ r ⁇ 1 ⁇ m, and from the tip to the vicinity of the needle tip 8
- the opening angle of the cone when ⁇ is approximated as a part of the cone 9 is defined as ⁇ , 5 ° ⁇ ⁇ (8 / r) °.
- the unit of r is ⁇ m.
- FIG. 2 shows a schematic diagram of an example in which the electron source 10 is applied to a scanning electron microscope (SEM).
- SEM scanning electron microscope
- an extraction voltage V1 is applied from an electron gun power source to generate probe electrons 5 having a desired current amount.
- the electron beam becomes a desired electro-optical condition by the acceleration voltage V0 and the first anode voltage V2, and is focused on the sample 24 by the electro-optical components mainly including the condenser lens 15 and the objective lens 23.
- This focal position is scanned by the deflector 19, and the detection electrons 15 generated from the sample are detected by the electron detector 16 via the ExB deflector 17 and converted into electrical signals, and an SEM image is obtained on the controller 28.
- low acceleration high resolution mode there are two types of operation functions: low acceleration high resolution mode and high-speed elemental analysis mode.
- the incident energy to the sample is 1 kV or less to 50 eV.
- This condition is useful for observing fine samples such as semiconductors and nanomaterials that are easily broken by charging or electron beam impact.
- the image blur due to chromatic aberration: dc is proportional to the electron beam energy width: ⁇ E, and is inversely proportional to the electron energy passing through the objective lens 23: Vobj, and becomes dc ⁇ E / Vobj.
- a voltage Vb for accelerating electrons is applied to the booster electrode 20 placed above the objective, and simultaneously, a retarding voltage Vs for decelerating electrons is applied to the sample 24 from the power source 27.
- V0 -3kV
- Vb + 1kV to + 5kV
- the first anode 12 between the two electrodes adjusts the lens action that occurs when the potential difference between the two is large.
- the extraction electrode 11 is at a positive potential and it is necessary to greatly decelerate toward the second anode, a large aberration occurs due to the deceleration electric field.
- the brightness of the electron source originally generated from the electron source 1 is reduced by the deceleration. Therefore, the greater the deceleration, the worse the final resolution.
- V0 + V1 is 0 or negative. This is a condition that the absolute value of the extraction voltage V1 is equal to or smaller than the absolute value of the acceleration voltage V0. Therefore, it is desirable to set the practical upper limit of V1 to 3 kV in the low acceleration high resolution mode.
- the required time is given priority over the resolution in many cases. This is because, in SEM, secondary electrons and backscattered electrons can be obtained in the same order as the probe electron beam 14, so these can be measured with high sensitivity and at high speed, but compared to this, X-rays are generated. This is due to the small amount. Therefore, it is desirable to irradiate the probe electron beam 14 as much as possible as compared with the high resolution observation.
- the electron energy of the sample is made low, for example, 4 kV, and the generated X-ray energy distribution is measured by the X-ray analyzer 21 with a resolution of about 3 nm.
- Vs 0V
- the maximum effect is obtained when V1 is used at 4 kV or less.
- the amount of probe current is V0 / V1 times the radiation angle current density J0 (A / sr) emitted from the electron source 1, so that the desired radiation angle current is as low as V1. It is desirable that the density is obtained, and V1 is 4 kV or less.
- FIG. 5A shows an example of the relationship between the surface electric field E and the extraction voltage V1.
- the extraction voltage V1 is a value used in the apparatus of FIG.
- the horizontal chain lines A and B represent the electric fields necessary for the low acceleration high resolution mode and the high speed elemental analysis mode, respectively.
- the unit of r is ⁇ m, and the unit of ⁇ is °.
- the reason for such a curve is that when the tip radius of curvature r is different, the electric field is also different.
- ⁇ ⁇ (8 / r) is obtained.
- the initial velocity of electrons emitted from the electron source is small, when the current density exceeds a certain level, there is a phenomenon that the energy width and the light source size are remarkably increased due to repulsion due to Coulomb interaction between electrons. This is called the space charge effect or the Boersch effect.
- the current discharged per unit solid angle and the radiation angle current density J (A / sr) are used as parameters of the amount of current emitted from the electron source. Note that an index indicating luminance is obtained by dividing J by the light source size S (m 2 ).
- the value J / S is proportional to the acceleration voltage
- the value J / S / V0 divided by the acceleration V0 may be used as reduced brightness.
- the light source size S increases substantially in proportion to r 2. Therefore, when the same luminance is to be obtained, the radiation angle current density J must also be increased in proportion to r 2 .
- the boundary where this effect becomes significant is indicated by a solid line in FIG. In the upper left of this, the space charge dominant region 30 having dots is a region where the space charge effect is dominant and is clearly undesirable.
- the solid line in FIG. 3A is determined as follows.
- FIG. 3B plots the energy width (half-value width) ⁇ E of the electron beam with respect to J for each tip curvature radius r.
- ⁇ E the energy width (half-value width) of the electron beam with respect to J for each tip curvature radius r.
- the cases where r is 0.55 ⁇ m and 0.8 ⁇ m are also plotted.
- this ⁇ E exceeds approximately 1 eV, the space charge effect becomes prominent, and the energy width and the light source size rapidly deteriorate. Therefore, a plot of J and R at this time is the boundary line in FIG.
- r should be larger than 0.5 ⁇ m. If a larger current is required, the hatched region 31 shown in FIG. 3A may be selected from the region 31 where the space charge effect is small. Therefore, r is preferably larger than 0.5 ⁇ m.
- the energy width of the electron beam from the SE electron source at the same surface electric field E is basically the same even if r is different, and the current density is also the same.
- What differs depending on r regarding the characteristics of the light source is the area of the emission source in addition to the extraction voltage V1.
- J increases in proportion to the area, but the size of the electron light source also increases. Increase As a result, the probe current decreases with the reduction in the electron optical system.
- the surface electric field E is the same, substantially the same probe current can be obtained even if r is different.
- ⁇ at the tip of the electron source when it is 5 ° or less, there is a problem that when the diameter is continuously changed as shown in FIG. 1B, the elongated portion of the tip becomes too long.
- FIG. 1 (c) electrons emitted from the W (100) plane formed at the tip of the needle are used, but an equivalent plane appears in the vertical direction, and these are four-fold symmetric around the central beam. Results in a release pattern. There are a total of four vertical planes (010), (001) and their opposite planes. If these areas are much larger than the (100) plane of the tip, Flares are mixed in the probe electron beam 14 used in such an apparatus, and it becomes difficult to focus on a fine beam.
- the area of this side surface depends on ⁇ , and the smaller ⁇ is, the longer the (010) and (001) planes become, and thus the larger the side surface area becomes. For this reason, in order to suppress flare, ⁇ > 5 ° is desirable. From the above, 0.5 ⁇ m ⁇ r ⁇ 1 ⁇ m and 5 ° ⁇ ⁇ (8 / r) ° are suitable as conditions for achieving both low acceleration and high resolution performance and a high-speed elemental analysis function. This is the preferred condition region shown in FIG.
- ⁇ 8 to 11 °
- the radiation angle current density can be used at 0.4 mA / sr. Therefore, high-speed EDX analysis and radiation angle current ⁇ 30 ⁇ A
- the aperture By setting the aperture to / sr and ⁇ E to 0.4 eV, a resolution of 1.2 nm can be obtained even at a low acceleration of about 800 eV. Low-acceleration, high-resolution observation and high-speed analysis are possible with a single electron beam device.
- the W single crystal rod 7 is electrolytically etched to form a tip needle, and then heated in a vacuum to round the tip to obtain a desired shape.
- the most typical method is to immerse the W single crystal rod 7 in an aqueous solution of about 1 mol / L of NaOH or KOH, pass an electric current through the rod, electrolytically etch the portion in the liquid, and stop at an appropriate place. Leave the shape. If a direct current is used at this time, a shape in which the opening angle becomes smaller as going to the tip as shown in FIG. 1B is obtained, which is convenient for making a tip having a small ⁇ .
- a conical shape having a substantially constant opening angle can be obtained, which is advantageous for forming a 12-16 ° region where ⁇ is large.
- the surface is slightly polished using an alternating current to adjust the ⁇ to a desired size.
- W can be prevented from evaporating, so that the heating temperature can be increased and the process time can be shortened.
- a halogen gas such as H 2 gas, F 2 , or Cl 2
- W can be prevented from evaporating, so that the heating temperature can be increased and the process time can be shortened.
- a filament for heating the tip
- another electron source may be placed nearby, and the W needle may be irradiated with the electrons from here to heat. For this, light may be collected and heated even if it is not electrons. This may be achieved by forming an optical system using a lens or a condensing mirror so as to focus in the vicinity of the tip of the needle in a vacuum.
- the tip portion of the needle with a small r formed by electrolytic etching or the like is removed with a focused ion beam (FIB) or the like, and the amount of movement of W atoms is reduced. It is to be.
- FIB focused ion beam
- FIG. Needle formed by etching The opening angle ⁇ used in FIG. 7 (a) is a value obtained when the diameter ⁇ of the cross section of the tip 8 is about twice the required r. Decide on.
- Ga + is widely used as an ion beam.
- the heating condition may be about 1800K for 1 hour or 2100K for 5 minutes, for example.
- FIB processing is performed on W immediately after etching, but FIB processing is also effective after a Zr—O diffusion source is attached as an electron source as shown in FIG.
- a Zr—O diffusion source is attached as an electron source as shown in FIG.
- the heating in vacuum for obtaining the desired r may be performed before and after electron emission in a state of being put in an electron gun. In this case, an extra step of heating in vacuum can be omitted.
- Any ion species other than Ga may be used as long as it has an etching action. For example, oxygen ions and Ar ions may be used.
- EDX was used as the X-ray detector, but WDX that measures chromatic dispersion may be used.
- low acceleration electrons of 4 kV are used, if the signal can be detected, the incident energy of the electron beam may be used in the range of 3 kV to 15 kV. When the electron energy is large, the number of X-ray signals increases, so that high-precision and short-time detection can be performed.
- FIG. 8A shows one electron source according to an embodiment of the present invention.
- the portion from which electrons are emitted is a needle-like tip 8 provided at the tip of the W single crystal rod 7, and a heating element 104 made of W filament is energized and heated from the diffusion source 102 to the metal sintered body 100 to Ba—O.
- the oxide containing is impregnated.
- These components are housed in a cathode support tube 105, and a cathode cap 106 is fitted to prevent the metal sintered body 100 from falling off and to control the oxygen partial pressure.
- the main component of the sintered metal 100 is W, and the Ba and O atoms generated by reduction are diffused on the surface of the W single crystal rod, and a low work function surface of Ba—O—W is formed at the needle tip 8.
- the electron beam is emitted from here. Electric power to the heating element 104 is supplied through the two electrodes 4.
- the temperature of the tip 8 is in the range of 800K to 1200K. More preferably, when operated in the range of 1000K to 1100K, an electron source having both monochromaticity and stability can be obtained. This operating temperature can be confirmed with a radiation thermometer from the outside through one of the holes 109 formed in a part of the suppressor 6. Alternatively, a thermocouple may be placed inside. The current, voltage, or power consumption of the heating element 104 is controlled so that the measurement temperature becomes a desired temperature.
- a suppressor electrode 6 is provided, and the position of the cathode support cylinder 105 is fixed using a set screw 108 via the cathode insulator 103. .
- the lifetime of the diffusion source 102 is determined where Ba can no longer be supplied, and in order to extend this lifetime, the capacity of the diffusion source 102 must be increased and evaporation in the vacuum must be prevented.
- the cathode support tube 105 and the sintered metal body 100 are covered so that they do not easily evaporate, and the capacity can be selected to a desired size. Is characterized by a lifetime of more than 5 years.
- the oxide containing Ba-O when only the oxide containing Ba-O is used as a diffusion replenishment source, there is a disadvantage that when it is placed in the atmosphere, it absorbs moisture and becomes BaOH, which causes deterioration of electron source characteristics. Since the rate of deterioration can be slowed by covering with the metal sintered body 100 as in the structure, the deterioration can be prevented and handled. For example, if it is sealed in dry nitrogen during storage, it can be stored for more than one year without deterioration. When actually used, it is opened and taken out to the atmosphere, and there is no deterioration even in the work for 1 to 2 hours in the atmosphere. Furthermore, even if the product is once used as an electron source and then taken out into the atmosphere, it can be used without deterioration for about one year by storing it in an atmosphere free from moisture such as dry nitrogen.
- a metal powder compact 101 is provided at one end of the W ⁇ 100> single crystal rod 7. This is formed by placing W powder (average particle size 0.5-3 ⁇ m) in one end of a W single crystal rod. About 1% as a binder, higher alcohols such as isostearyl alcohol may be added. The diameter of the W single crystal rod is about 0.13 mm, and the W powder portion has a diameter of about 0.5 to 5 mm and a height in the range of 0.5 to 5 mm. This is calcined at 1000K or higher in hydrogen or vacuum to evaporate the binder, heated at 2000K ⁇ 200K for 5 minutes to 1 hour and sintered.
- a needle-shaped tip 8 is formed by an electrolytic etching method using a NaOH aqueous solution or a KOH aqueous solution (FIG. 8C). ).
- the sintered metal 100 is porous, and a porosity of about 1 to 20% is desirable.
- Ni or the like may be added as a metal.
- an alloy containing Mg, Si, etc. in the range of 0.05 to 0.25% as a main component of Ni may be used.
- the diffusion source 102 is mainly a mixture of BaO, CaO, and SrO. These may be prepared in advance by molding Ba carbonate, Ca carbonate, and Sr carbonate powder, and heated to 1000K or higher to form oxides by thermal decomposition. When a binder is added, moldability is good. For example, about 1 to 10% of an alcohol or ether solution of collodion is preferably added. Once an oxide is formed, it will deteriorate due to moisture absorption in the atmosphere, so it must be stored in dry air, nitrogen, or vacuum. Alternatively, it is possible to attach the carbon dioxide as it is, decompose it into an oxide by heating, and use it as an electron source without removing it.
- a diffusion source not only an oxide but also a compound that liberates Ba by heating or a reduction reaction, such as barium chromate (BaCrO 4 ) or barium manganate (BaMnO 4 ), may be used.
- barium chromate BaCrO 4
- BaMnO 4 barium manganate
- getter material grains are mixed in these materials. May be.
- the getter material adsorbs oxygen and hydrogen and refers to, for example, an alloy mainly composed of Zr, Ti or the like.
- a metal mainly composed of Zr or Ti may be used for the sintered metal 100.
- the suppressor electrode is used in order to prevent the generation of extra thermoelectrons, but it is sufficient that there is one having an electron potential higher than the energy of the thermoelectrons from the surface of the sintered metal 100.
- the cathode cap 106 may be lengthened.
- the work function is 4.5-5 eV, and it comes out from the central part of the W surface where the work function is lowered to 2.0 or less. Since the energy of the coming electrons is 2 eV or more lower than the vacuum level of the hole of the cathode cap 106, it is pushed back to a lower potential portion.
- the opening of the central hole 110 needs to be sufficiently narrow compared to the length of the hole.
- a degassing hole 111 may be provided in the cathode cap 106 as shown in FIG. 9B in order to quickly let out the emitted gas from the Ba diffusion source 102 and the sintered metal body 100.
- the energy width is 0.2 to 0.3 eV and can be used under the condition of about 1/2 to 1/3.
- the electron source 1 in the diagram used in Example 1 chromatic aberration is reduced and high resolution is achieved. A resolution of about 0.8 nm can be obtained at a sample incident energy of 1 kV.
- the work function is low, an electric field applied to the surface of the electron source emits a larger current when the electric field is lower than before, so that there is an advantage that X-ray analysis can be performed in a shorter time.
- the energy width of 0.2 eV is better in monochromaticity than the field emission (FE) electron source using W ⁇ 310>, so the electron optical system used at a reduced speed achieves higher performance by using the electron source of this embodiment. Is done. For example, when applied to a low-speed electron microscope (LEEM) or a mirror-type electron microscope, not only higher resolution but also an image signal amount increase, so that high-speed observation is possible with the same resolution.
- LEEM low-speed electron microscope
- a mirror-type electron microscope not only higher resolution but also an image signal amount increase, so that high-speed observation is possible with the same resolution.
- the tip shape of the electron source is effective when 0.5 ⁇ m ⁇ r ⁇ 1 ⁇ m and 5 ° ⁇ ⁇ (8 / r) ° as in Example 1, but the work function is low and the required electric field is small. Is effective up to about 3 ⁇ m and ⁇ up to 30 °.
- a smaller r for example, 0.2 to 0.5 ⁇ m and a small ⁇ of 5 to 10 ° can be used as a high brightness monochromatic electron source. Gives the best performance.
- the metal sintered body 100 and the diffusion source 102 are separately provided as the diffusion replenishment source. However, they may be manufactured as a single unit from the beginning, for example, as shown in FIGS. 10 (a) and 10 (b).
- a Ba diffusion replenishment source 112 provided in a part of the W single crystal rod 7 is obtained by impregnating an oxide containing Ba—O as a Ba diffusion source 102 in a gap between grains of the sintered metal 100. Also good.
- the electron source can be configured with the structure as shown in FIG. 10A, there are advantages such as a small number of components, small size, and low cost.
- a Ba diffusion source 102 may be wrapped with a sintered metal body 100 as shown in FIG.
- heating means for the W needle 1 serving as the electron emission source and the diffusion replenishment source there is one heating means for the W needle 1 serving as the electron emission source and the diffusion replenishment source, but there may be a plurality of heating means.
- W heating element 3 is connected to F1 and F2
- W needle 1 is heated
- replenishment source heating means 113 is connected to F2 and F3, Ba diffusion
- the supply source 112 is heated.
- the Ba diffusion supply source for example, a Ba diffusion source 102 impregnated with an oxide containing Ba—O is used in the gaps between the grains of the sintered metal 100.
- replenishment source heating means 113 a W filament is used, and the metal sintered body 100 and the electrode bar 4 are fixed by spot welding.
- the current If is passed for heating the W heating element 3, and the current Id is used independently for heating the replenishment source heating means 113.
- a constant current circuit is used here, the effect is the same for a constant voltage circuit, a constant power circuit, or the like as long as it can be heated to a desired temperature.
- Ba and O are evaporated and adsorbed on the surface of the W needle 1. This heating temperature can be confirmed from the outside through the hole 109 on the side surface of the suppressor 6 by the amount of emitted light or the color of emitted light.
- the W needle 1 is kept at a temperature between 900K and 1100K and emits electrons.
- the W needle 1 since it can operate as an electron source under the optimum conditions of both temperatures, there is an advantage that a stable one can be obtained with high brightness of a single color.
- the current amount of the W heating element 3 is temporarily increased, and the W needle 1 is increased from 1800K to 2200K. The surface can be cleaned by heating.
- the electrode 4 has four electrodes F1, F2, F3, and F4, the replenishment source heating means 113 is connected to F3 and F4, and a voltage is applied between F2 and F3. If Vd is applied, if the value of Vd is adjusted to about +10 to +300 V so that the replenishment source heating means 113 has a positive potential from the W needle 1, the thermoelectrons generated from the replenishment source heating means 113 will be W Since the inflow to the needle 1 and the W heating element 3 can be prevented, stable electron emission can be obtained.
- the supply source heating means 113 is generated from the supply source heating means 113 when Vd is set to about ⁇ 100 V to ⁇ 500 V so that the supply source heating means 113 has a negative potential with respect to the W needle 1.
- the W needle 1 can be heated by the thermoelectrons.
- the gap between the grains of the sintered metal 100 is impregnated with an oxide containing Ba—O as the Ba diffusion source 102.
- the same effect can be obtained even if the metal sintered body 100 is diffused and the cathode support tube 105 is used.
- an electron source suitable for an electron beam apparatus capable of low acceleration and high resolution and high-speed elemental analysis can be obtained.
- a charged particle beam apparatus is realized.
- Electron source 11 ... Extraction electrode, 12 ... First anode, 13 ... Second anode, 14 ... Probe electron beam, 15 ... Condenser lens, 16 ... Electron detector, 17 ... ExB deflector, 18 ... Detection electron , 19 ... Deflector, 20 ... Booster electrode, 21 ... X-ray analyzer, 22 ... Vacuum container, 23 ... Objective lens, 24 ... Sample, 25 ... Sample stage, 26 ...
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Abstract
Description
また、Ba-Oを含む酸化物を拡散源としたSE電子源では、動作を1000K程度に低温化すると電子放出が安定せず、連続で1ヶ月程度までしか使用できない等の安定性に問題があった。
本発明の主眼は、低加速で高分解能なSEM像を観察する場合に有用な金属焼結体とBa酸化物を含むBa拡散源から構成するSE電子源である。
図1(a)は、電子放出源となるW針1とそれを支えるWフィラメントによる発熱体3とZr-Oの拡散源2を持ち、これらがガイシ5と電極4上に保持され熱電子発生を抑えるサプレッサ6が被せられており、このW針(単結晶W金属針)1の針状先端8は、図1(b)のようにW単結晶棒円筒形から徐々に細くなって先端につながる部分(ここで、この部分を便宜的に「くびれ部」と呼ぶことにする)であり、この長さLnは針の強度を保つためと拡散距離が適度に短くなるように200μm以下が望ましい。さらに、先端部分の微細構造は先端を半球形に近似したときの球の半径を、先端の曲率半径rと呼び、このrは0.5μm<r<1μmであり、先端から針状先端8の近傍を円錐形9の一部として近似したときの円錐の開き角(opening angle)をαと定義したとき、5°<α<(8/r)°となる。ただし、rの単位はμmの条件である。先端付近で近似する円錐形状が曖昧な場合は、このαのより教義な定義として、図1(c)に示すように、先端からの距離3rから8rの間の領域を円錐形9として近似すればよい。
電子源10のサプレッサ電極6の下端面に引出電極11があり両者の間隔は0.7mm程度であり、電子源の針先端8サプレッサ6の下面から、0.2-0.3mm程度引出電極側につきだしている。ここに電子銃電源より引出電圧V1を印加して、所望の電流量のプローブ電子5を発生させる。この電子線は、加速電圧V0及び第1アノード電圧V2により所望の電子光学条件となって、コンデンサレンズ15および対物レンズ23を主とする電子光学部品類により試料24上に焦点を結ぶ。この焦点位置を偏向器19によりスキャンし、試料から発生する検出電子15をExB偏向器17を介して電子検出器16で検出して電気信号に変換し、コントローラ28上でSEM像が得られる。
顕著になる境界を図3(a)中に実線で示す。これより左上、ドットの有る空間電荷支配領域30は空間電荷効果が支配的であり、明らかに望ましくない領域である。この図3(a)中の実線は、次のようにして決められる。例えば、r=0.25μmの先端径のSE電子源では、およそ0.1mA/srから空間電荷効果が顕著になり、エネルギー幅の増加と、光源径の拡大のため、分解能が悪くなる、プローブ電流が増加しない等の問題が出てくる。図3(b)には、各先端曲率半径r毎のJに対する電子線のエネルギー幅(半値幅)ΔEをプロットしたものである。他に、rが0.55μm、0.8μmの場合もプロットしてある。このΔEがおおむね1eVを超えると空間電荷効果が顕著になり、エネルギー幅と光源サイズが急速に悪化するので、このときのJとRをプロットしたものが図3(a)中の境界線である。実用上、高速なEDX検出やパターン検査には0.2mA/sr以上のプローブ電流の放射角密度が必要であり、この条件で空間電荷効果の作用が顕著になり領域の90%以下の電流密度で使用すると良い。0.2から0.3mA/srの領域を使おうとすれば、rは0.5μmを超えるサイズが良い。より大電流が必要であれば、図3(a)のハッチングの、空間電荷効果が小さい領域31から選べばよい。従って、rは0.5μmより大きい事が好適となる。
空間電荷効果がない条件においては、同一表面電界EでのSE電子源からの電子線のエネルギー幅はrが異なっても基本的に同じ、電流密度も同じである。光源の特性に関してrによって違うことは、引出電圧V1の他に、放出源の面積がある。
SEMのプローブ電流量が、放射角電流密度Jで制限されている場合、Jは面積にほぼ比例して増加するが、電子の光源サイズも同様に大きくなるので、実際に使う場合には縮小率を大きくする。この結果、電子光学系での縮小に伴いプローブ電流が減少するため、結果として、表面電界Eが同じであれば、rが違ってもほぼ同じプローブ電流が得られる。
しかし、電源の要求性能が厳しくなってくる。例えば、r=0.3μm、α=10°の場合の0.2mA/srと同等のプローブ電流を得ようとすると、r=1μm、α=30°の場合、1.8mA/srが必要となり、引出電圧を7kV以上にする必要があり、また全放出電流も1mA前後流れる。このような高圧大電流の電源は、さらに高安定性が求められるので、電源のコストが非常に大きくなる。また、エネルギー消費も増えるので、社会にとって望ましい方向ではない。
このため、フレアの抑制のためには、α>5°が望ましい。
以上のことから、低加速高分解能性能と、高速元素分析機能を両立させる条件として、0.5μm<r<1μmかつ 5°<α<(8/r)°が好適となる。図4に示す好適条件領域となる。
イオン種としてはGa以外でもエッチング作用があれば良く、例えば、酸素イオン、Arイオンなどを用いても同様である。
これにより、針先8迄の電気的接触が得られる。ここで、電子源の動作のためには、先端8の温度が、800Kから1200Kの範囲とする。より好適には、1000Kから1100Kの範囲で動作させると、単色性と安定性の両立した電子源が得られる。この動作温度はサプレッサ6の一部に開けた穴109のうちの一つを介して外部から放射温度計で確認することができる。
あるいは、内部に熱電対を置いても良い。測定温度が所望の温度となるように、発熱体104の電流、電圧、もしくは消費電力を制御する。
図8(b)に示すように、W<100>単結晶棒7の一端に金属粉成形体101を設ける。これは、W単結晶棒の一端にW粉(平均粒径0.5-3μm)を型に入れて形成したものである。バインダーとして1%程度、イソステアリルアルコールのような高級アルコールを添加しても良い。W単結晶棒の直径は約0.13mmであり、W粉体の部分は、直径0.5から5mm程度で、高さ0.5から5mmの範囲とする。これを水素中もしくは真空中で1000K以上で、か焼して結合剤を蒸発させ、2000K±200K程度で5分から1時間程度の加熱を行い焼結する。あるいは1000K以上で、か焼するにとどめても良い。これにより単結晶棒7と金属焼結体100の組合せが得られ、この後、NaOH水溶液、あるいはKOH水溶液を用いた電解エッチング法により針状に尖った先端8を形成する(図8(c))。
金属としては、Ni等を添加しても良い。あるいは、Wを主たる成分とする必要性はなく、例えば、Niを主たる成分として、Mg、Si等を0.05-0.25%の範囲で含む合金を用いても良い。
Claims (13)
- 電子発生源たる単結晶W金属針と、Zr-O拡散源と、発熱体と、サプレッサ電極とを持つSE電子源を備えた電子線装置において、
前記単結晶W金属針は、円柱形状と、該円柱形状の上端面に延伸して設けられ径が徐々に細くなるくびれ部分と、該くびれ部分に延伸して設けられたほぼ円錐形状とから構成される形状を有し、
前記円錐形状の電子を放出する部分の先端形状を半球形に近似し、該半球の曲率半径をrと定義したとき、前記先端形状の曲率半径rは0.5μm<r<1μmであり、
前記円錐形状の開き角をαと定義したとき、前記開き角は、5°<α<(8/r)°(ここで、rの単位はμmとする)であることを特徴とする電子線装置。 - 前記単結晶W金属針において、前記円柱形状と前記くびれ部分とが接する境界から前記円錐形状の先端までの長さをLnと定義したときに、Ln<200μmであることを特徴とする請求項1記載の電子線装置。
- 前記先端形状の曲率半径rが、0.55μm≦r≦0.7μmであり、前記円錐形状の開き角をαが、8°≦α≦12°であることを特徴とする請求項2記載の電子線装置。
- 電子発生源たる単結晶W金属針と、Ba拡散手段と、発熱体とを有するSE電子源を備えた電子線装置において、
前記Ba拡散手段は、多孔質の焼結金属とBa-Oを含むBa拡散源から構成されることを特徴とする電子線装置。 - 前記Ba拡散手段からの熱電子放射を抑制するサプレッサ電極を持つことを特徴とする請求項4記載の電子線装置。
- 前記Ba拡散手段は、金属焼結体にBaO酸化物を含むBa拡散源を含浸させたものであることを特徴とする請求項4記載の電子線装置。
- 前記Ba拡散源の外側に焼結金属を配したものをBa拡散手段としたことを特徴とする請求項4記載の電子線装置。
- 前記Ba拡散手段は、Ba拡散源上に金属焼結体を配し、前記単結晶W金属針を前記金属焼結体に結合した結合体であることを特徴とする請求項7記載の電子線装置。
- 前記焼結金属は、Wもしくは、Ni、Cr、Feを主成分とし、粒径が0.1~10μmの粉体を焼結したものであることを特徴とする請求項4記載の電子線装置。
- 前記Ba拡散源は、Ba-Oを含む酸化物でBaO単体、もしくはCaO、SrOあるいはBa、Ca、Srの炭酸化物を含むことを特徴とする請求項4記載の電子線装置。
- 前記Ba拡散源は、クロム酸バリウム(BaCrO4)、マンガン酸バリウム(BaMnO4)、あるいはこれらの混合物と、Zr、Tiを主成分とする合金の粒子を含むことを特徴とする請求項4記載の電子線装置。
- 電子線を放出する電子源と、
放出された前記電子線に偏向を与える偏向手段と、
試料に前記電子線を照射する照射手段と、
前記試料から発生する電子を検出する電子検出手段、あるいはX線を検出するX線検出手段のうち、いずれか少なくとも一つを有し、
前記電子源が、請求項1乃至3のいずれか1項に記載の電子線装置を用いて構成されていることを特徴とする電子線応用装置。 - 前記電子検出手段と前記X線検出手段の両方を備え、
前記X線検出手段は、波長あるいはエネルギーにより放出された電子線を分類する機能を有することを特徴とする請求項12記載の電子線応用装置。
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Also Published As
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US20110240855A1 (en) | 2011-10-06 |
JPWO2010070837A1 (ja) | 2012-05-24 |
JP5166551B2 (ja) | 2013-03-21 |
DE112009003724T5 (de) | 2012-07-05 |
US8450699B2 (en) | 2013-05-28 |
DE112009003724B4 (de) | 2017-07-13 |
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