The present invention relates to a method for manufacturing an electron source, and relates to a method for adjusting the diameter of a tip end, serving mainly as an electron source, to have a desired size. The thus processed tip is used for equipments that operate with electrons extracted into vacuum, such as electron microscope, electron beam application device such as electron beam lithography system, probe microscope such as Scanning Tunneling Microscope (STM), in which the tunneling current is used, and Atom Force Microscope (AFM), in which the atom force is used, and in other way ion microscope in order to observe, manufacture and inspect the specimen.
When intense electric field is applied to the surface of metal, potential level is inclined at the vacuum. Then when the electric field exceeds the order of 109 V/m, the potential barrier becomes extremely thin, so that electrons are emitted into vacuum due to the tunneling-effect. This is called field emission. When intense electric field with the order of over 108 V/m is applied to the surface of heated metal, the Schottky effect occurs, and then electrons are emitted into vacuum. Recently as the electron source of a high-resolution electron microscope, a field-emission electron source based on the field emission phenomenon (Cold Field Emitter: CFE) and a Schottky electron source based on the Schottky effect (Schottky Emitter: SE) are mainly used.
In order to emit an electron beam from an electron source, such as CFE and SE, the diameter of the electron source at the tip end has to be thin in the nanometer order because sufficiently intense electric field is applied to the tip end. Conventionally a typical electron source is manufactured by sharpening a metal thin wire at the end by electrolytic polishing. Electrolytic polishing is a technique to sharpen the metal wire in electrolyte, applying voltage for electrolysis to melt the metal wire. In case of using SE, it is required to have a proper diameter of electron source at the tip end according to the property such as the amount of the beam current, the width of the beam energy, the stability of the beam and so on. And as other methods to sharpen the wire, there are various methods such as heat-treating, dry etching and ion etching in order to have the desired diameter.
JP H11-31453 A, for example, discloses a method of manufacturing a tip by electrolytic polishing. JP H08-36981 A discloses a method of heat-treating of a sharpened thin wire, dry etching, and etching by the ions which are ionized gas by electrons, which are emitted from tungsten monocrystal wire by applying voltage as a cathode. JP 2008-177017 A discloses a method of processing a tip end by FIB.
Patent Literature 1: JP H11-31453 A (U.S. Pat. No. 5,993,636)
Patent Literature 2: JP H08-36981 A
Patent Literature 3: JP 2008-177017 A
There is a need for analysis of compositions and components of a specimen these days in the field of electron microscopes. Such an analysis needs to focus a large current on a specimen, meaning that the large current has to be emitted from an electron source. A conventional electron source having the diameter of 0.8 μm or less at the end is good for high-resolution observation of a specimen with a small current. For emission of the larger current, however, it has problems of an increase in chromatic aberration resulting from the wider energy width and of poor current stability, and so fails to emit with a large current.
Then, a thick electron source having the diameter at the end of 0.8 μm or more is devised as the electron source for analysis. Such an electron source can have widen emission site of electrons, and can minimize the electrons interaction, and emit a large current while decreasing the energy width.
Then a method of controlling the diameter of the tip end is required. The aforementioned methods, however, have the following problems. That is, the method of the electrolytic polishing yields a diameter at the tip end in the nanometer order, which is too small for electron sources. In the method of heat treating, the shape of the tip end after electrolytic polishing affects the diameter at the tip end, and a size error is quite large. In the methods of dry etching and ion etching, the diameter at the tip end is not controlled, meaning that a tip cannot be manufactured by designating the size, and so a tip having a desired diameter cannot be acquired. When the tip end is precisely-processed by FIB, impurities may be attached to the tip, and so these methods cannot be used.
In order to fulfill the above object, current is allowed to flow through a heating element in vacuum to heat a tip, and negative voltage relative to the electrode disposed in front of the tip is applied to the tip to process the tip end. Herein, based on a substantially proportional relationship between the voltage and the diameter at the end, the voltage is controlled to have a desired diameter at the end, whereby the tip end is adjusted for processing. Then, heat treatment may be performed after this processing, whereby crystal defects occurring at the tip end or the surface roughness during processing may be corrected, and the tip end can be controlled in size to have a diameter at the end that is larger than that manufactured only by this processing.
While a conventional technique fails to manufacture a tip having a designated diameter at the end, the present invention as stated above can manufacture a sharpened tip made of a tungsten monocrystal thin wire to have any desired diameter in the range from 0.1 μm to 2.0 μm. Since this manufacturing method does not include FIB, impurities are not attached to the tip.
The following describes embodiments of the present invention, with reference to the drawings. In the present invention, a tip is processed by a method in which a change in current over time that is emitted from the tip end is monitored during the processing of the tip at the end, and voltage is increased so as to the voltage corresponding to a desired diameter of the tip end and then the processing is stopped in appropriate processing time.
Embodiments of the present invention are described below, with reference to the drawings.
As illustrated in
Embodiment 1
The vacuum vessel 4 is evacuated to the pressure from about 10−4 Pa to 10−2 Pa, and the major component of the residual gas is water. In the present embodiment, a tip can be easily processed without the necessity of introducing gas for processing especially, and another gas may be introduced if ions can be generated for the processing of a tip, where the type of the gas may be selected. Although the pressure may be in the low-vacuum state of 10−2 Pa or more, such pressure may cause discharge that leads to ionization of the residual gas like avalanche. Although the pressure may in the high-vacuum state of 10−4 Pa or less, such pressure decreases the possibility of ionization of the residual gas, which may lead to the possibility that the processing of a tip end does not progress. In this way, the pressure from 10−2 to 10−4 Pa is conceivably optimum for processing of a tip.
Current is allowed to flow through the heating element 2 to heat the tip 1 in the range from 1,500 K to 2,000 K. Such temperatures do not change the atomic structure of the inside of the tip 1, but allows atoms at the surface of the tip at the end only to move, which is called atom migration. At the temperatures of 1,500 K or less, the emission current is small so that the processing may not progress, and at the temperatures of 2,000 K or more, atoms at the surface of the tip at the end move a lot, causing a change in diameter at the tip end and so it is difficult to control the diameter. In this way, the range of 1,500 K to 2,000 K is conceivably appropriate for processing. The appropriate temperature range may vary with the material of a tip, and so appropriate temperatures have to be investigated for a tip made of another material so as to allow atoms at the surface to move without changing the atomic structure.
When negative voltage relative to the extraction electrode 3 is applied to the tip, electric field is generated around the tip 1.
Js: Current density, me, k, j, e, ε0: Physical constants, ϕ: Work function, F: Electric field intensity, T: temperature
Out of the residual gases ionized, residual gas 34 positively ionized collides with the tip end 31 to grind the surface of the tip and so round the tip end.
When the tip is ground and the tip end becomes round, then the electric field around the tip is weakened, and so the electric field concentrated on the surrounding of the tip is weakened.
When the electric field applied around the tip is weakened, the number of electrons emitted by field emission decreases in an exponential manner as is expected from expression 1, and so the current emitted from the tip decreases, and the electric filed is weakened. This means a decrease of the residual gas ionized, and so the number of ions colliding with the tip decreases.
Since the tip is heated to move atoms at the surface, the ground part of the tip by the collision will be filled with the atoms. The rate of grinding of the tip surface by ions and the rate of filling of the ground part by the movement of atoms at the surface reaches the equilibrium state, and then the tip has a shape of a certain thickness. At this time, the electric field around the tip does not change apparently.
Then the relationship between the voltage and the diameter at the tip end at this time is investigated, and the result is as illustrated in the graph of
Further a change over time in sum of the current emitted from the tip end and the current due to residual gas ionized is monitored during the processing of the tip end.
A change in current over time is monitored in this way because of the following two reasons. Firstly, if high voltage is applied suddenly to the tip end when the diameter at the tip end is still small before the grinding, then discharge may occur in such a manner that residual gas is ionized like avalanche. When the applied voltage corresponding to the diameter at the tip end exceeds 2 kV, the voltage has to be increased in a step-by-step manner so as not to increase the current too large, and after confirming that the diameter at the tip end is large enough to avoid the discharge, then the voltage may be increased. In the present embodiment, the voltage is increased in a step-by-step manner so as to keep the current at 50 μA or less. Secondly, monitoring of a change in current over time allows an operator to know indirectly that the processing at the tip end starts when the current increases, and that the processing at the tip end reaches its final stage when the current decreases and becomes constant and is in the equilibrium state. That is, although a change in diameter at the tip end cannot be known during the processing of a tip in conventional techniques, the monitoring of current allows an operator to know the progress of the processing of the tip end, and enables visualization of a change in diameter at the tip end.
In Embodiment 1, the processing time is set until the current becomes constant. However, the processing rate is substantially constant irrespective of individual differences of tips, and so the processing time may not be limited to the time until the current becomes constant. The processing time may be set at any time, and a graph similar to
Embodiment 2
Electrolytic polishing is a technique of soaking a thin wire into electrolyte solution, followed by application of voltage, thus fabricating a sharpened tip end, and at this time, the tip end has a different shape between DC voltage and AC voltage applied (hereinafter polishing by DC voltage is called DC electrolytic polishing, and polishing by AC voltage is called AC electrolytic polishing). When a tungsten monocrystal thin wire having axial orientation of <100> is polished, the resultant tip end has a different angle at the conical part (cone angle) between the DC electrolytic polishing and the AC electrolytic polishing.
When a tip having the cone angle of 10° or less is used as an electron source, deformation of the tip end due to atoms moving at the surface is less, meaning good stability of the emission current. When the cone angle is small, electric field generated around the tip easily is concentrated on the tip when voltage is applied to the tip. That is, this has advantages that a power supply of small capacity is enough to emit a certain amount of current and problems about discharge with another component hardly occur.
When the cone angle is large, the diameter at the tip end easily changes, meaning poor stability of emitted current.
That is, a thin wire sharpened by DC electrolytic polishing can have a cone angle that is freely set at a small size, and the thus obtained thin wire by electrolytic polishing may be processed by the method similar to Embodiment 1, whereby a tip having a small cone angle and having high stability for emitted current can be processed to have a desired diameter at the tip end of 0.1 to 2.0 μm.
Embodiment 3
Although the processing time of a tip is set at a certain time in the method of Embodiment 1, the processing time may be used as a parameter to control the diameter at the tip end while setting the applied voltage constant.
Embodiment 4
When intense electric field is applied to the tip end in the method of Embodiment 1, discharge may occur. Actually a tip was broken due to discharge when the processing was performed at 7 kV or more. Then, countermeasure for discharge is required when intense electric field is applied. A generally known method of processing the tip end is heat treatment, and then a tip was processed by a method including heat treatment in combination with the method described in Embodiment 1. In this embodiment, heat treatment was performed at part C of
Too high temperatures of heat treatment in this case increase a change of the shape per unit time, and so can shorten the processing time. However, it becomes difficult to control a change of the shape with a high precision. Conceivably a temperature of the heat treatment that is higher than the temperatures used in Embodiment 1 and is in the range from 2,000 K to 2,500 K can control the ratio of increasing the diameter of a tip end for processing. Herein since the time and the temperature of heat treatment depend on the material of a tip, they may be investigated for a material other than tungsten for setting.
Embodiment 5
When the heating element is heated for heat treatment of a tip, the heating element is worn unfortunately. To avoid this problem, the tip may be heated through thermal electrons using a filament 81 that is disposed around the tip.
Embodiment 6
Herein, the tip may be selected so that, when the current of a primary electron beam may be about a few pA due to conditions to observe and analyze the specimen 207, the diameter of the tip at the end may be 800 nm or less, and when large current of a few nA or more is required for low chromatic aberration and high stability, the diameter of the tip at the end may be of a desired size of 800 nm or more.
Filing Document | Filing Date | Country | Kind |
---|---|---|---|
PCT/JP2012/076381 | 10/12/2012 | WO | 00 |
Publishing Document | Publishing Date | Country | Kind |
---|---|---|---|
WO2014/057570 | 4/17/2014 | WO | A |
Number | Name | Date | Kind |
---|---|---|---|
5993636 | Terui et al. | Nov 1999 | A |
20110240855 | Ohshima | Oct 2011 | A1 |
20120269326 | Adler | Oct 2012 | A1 |
Number | Date | Country |
---|---|---|
8-36981 | Feb 1996 | JP |
08036981 | Feb 1996 | JP |
2789610 | Aug 1998 | JP |
2789610 | Aug 1998 | JP |
10-255703 | Sep 1998 | JP |
10255703 | Sep 1998 | JP |
11-31453 | Feb 1999 | JP |
2005-339922 | Dec 2005 | JP |
2008-177017 | Jul 2008 | JP |
2008-293844 | Dec 2008 | JP |
2009-301920 | Dec 2009 | JP |
2011-124099 | Jun 2011 | JP |
Entry |
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International Search Report (PCT/ISA/210) dated Nov. 20, 2012 with English translation (five pages). |
Japanese-language Written Opinion (PCT/ISA/237) dated Nov. 20, 2012 (four pages). |
Chinese-Language Office Action issued in counterpart Chinese Application No. 201280076337.X dated Sep. 13, 2016 (6 pages). |
Number | Date | Country | |
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20150255240 A1 | Sep 2015 | US |