Electron source and electron beam device using the same
10707046 ยท 2020-07-07
Assignee
Inventors
- Toshiaki KUSUNOKI (Tokyo, JP)
- Keigo KASUYA (Tokyo, JP)
- Takashi OHSHIMA (Tokyo, JP)
- Tomihiro HASHIZUME (Tokyo, JP)
- Noriaki ARAI (Tokyo, JP)
- Yoichi OSE (Tokyo, JP)
Cpc classification
H01J37/073
ELECTRICITY
H01J37/20
ELECTRICITY
International classification
H01J37/073
ELECTRICITY
Abstract
An electron source that can be used stably for a long time even when hexaboride is used, and an electron beam device using the electron source are provided. The invention is directed to an electron source which includes a filament made of a metal, a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery, and a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is in contact with a bottom of each of the plurality of recesses of the metal tube.
Claims
1. An electron source comprising: a filament made of a metal; a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery; and a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is in contact with a bottom of each of the plurality of recesses of the metal tube.
2. The electron source according to claim 1, wherein the metal tube is joined to the filament by spot welding.
3. The electron source according to claim 1, wherein the metal tube has a plurality of other recesses at other positions of the metal tube in the axial direction, in addition to the plurality of recesses.
4. The electron source according to claim 1, wherein the hexaboride tip has a square pole shape, and the plurality of recesses are formed in two axes and four directions with respect to the hexaboride tip having the square pole shape.
5. The electron source according to claim 1, wherein the hexaboride tip has a circular cylindrical shape, and the plurality of recesses are formed in three axes and three directions with respect to the hexaboride tip having the circular cylindrical shape.
6. The electron source according to claim 1, wherein the metal tube is made of tantalum or niobium.
7. The electron source according to claim 1, wherein an inner diameter of the metal tube is in a range of 1.1 to 1.5 times the largest diameter of the hexaboride tip.
8. The electron source according to claim 1, wherein a thickness of the metal tube is in a range of 100 to 200 m.
9. An electron beam device comprising: an electron source; a sample stand on which a sample is placed; and an electron optical system for irradiating a sample on the sample stand with an electron emitted from the electron source, wherein the electron source is the electron source according to claim 1.
10. An electron source comprising: a filament made of a metal; a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery; a graphite sheet or rhenium foil disposed inside the metal tube; and a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is in contact with the graphite sheet or rhenium foil disposed at the bottom of each of the plurality of recesses of the metal tube.
11. An electron beam device comprising: an electron source; a sample stand on which a sample is placed; and an electron optical system for irradiating a sample on the sample stand with an electron emitted from the electron source, wherein the electron source is the electron source according to claim 10.
12. An electron source comprising: a filament made of a metal; a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery; and a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is coated with glassy carbon or a mixture of glassy carbon and boride carbon and is in contact with the plurality of recesses of the metal tube.
13. An electron beam device comprising: an electron source; a sample stand on which a sample is placed; and an electron optical system for irradiating a sample on the sample stand with an electron emitted from the electron source, wherein the electron source is the electron source according to claim 12.
Description
BRIEF DESCRIPTION OF DRAWINGS
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DESCRIPTION OF EMBODIMENTS
(25) As a result of investigations by the inventors, it was found that, particularly when manufacturing a field emission electron source of hexaboride or a thermal field emission electron source of hexaboride, a more robust and reliable joining in which a tip does not fall off even when the electron source is heated for a long time can be achieved by providing a plurality of recesses from at least two axial directions so as to surround a central axis of a metal tube made of tantalum or niobium and a hexaboride tip disposed inside thereof, at an outer periphery of the metal tube and bringing respective bottoms of the plurality of recesses into contact with an outer periphery of the hexaboride tip, respectively. More preferably, it was found that a plurality of recesses are also provided at points which are on the outer periphery of the metal tube and deviated in the axial direction of the metal tube and the bottoms of the respective recesses are in contact with the outer periphery of the hexaboride, respectively, thereby capable of obtaining a more robust joining without optical axis deviation.
(26) It was found that, particularly when manufacturing a thermal electron source of hexaboride or a Schottky electron source of hexaboride, a more robust and reliable joining can be achieved in which a tip does not fall off even when the electron source is heated for a long time by providing a plurality of recesses from at least two axial directions so as to surround a central axis of a metal tube made of tantalum or niobium, a hexaboride tip disposed inside thereof, and a graphite sheet or rhenium foil inserted therebetween, at an outer periphery of the metal tube and bringing respective bottoms of the plurality of recesses into contact with a graphite sheet or rhenium foil on an outer periphery of the hexaboride tip, respectively. More preferably, it was found that a plurality of recesses are also provided at points which are on the outer periphery of the metal tube and deviated in the axial direction of the metal tube and the bottoms of the respective recesses are in contact with a graphite sheet or rhenium foil on the periphery of the hexaboroid, respectively, thereby capable of obtaining a more robust joining without optical axis deviation.
(27) It was found that, particularly when manufacturing a thermal electron source of hexaboride or a Schottky electron source of hexaboride, a more robust and reliable joining can be achieved in which a tip does not fall off even when the electron source is heated for a long time by providing a plurality of recesses from at least two axial directions so as to surround a central axis of a metal tube made of tantalum or niobium, a hexaboride tip disposed inside thereof, and glassy carbon inserted therebetween, at an outer periphery of the metal tube and bringing respective bottoms of the plurality of recesses into contact with glassy carbon or a mixture of glassy carbon and boride carbon coating the outer periphery of the hexaboride, respectively. More preferably, it was found that a plurality of recesses are also provided at points which are on the outer periphery of the metal tube and deviated in the axial direction of the metal tube and the bottoms of the respective recesses are in contact with glassy carbon or a mixture of glassy carbon and boride carbon coating the outer periphery of the hexaboride, respectively, thereby capable of obtaining a more robust joining without optical axis deviation.
(28) Hereinafter, the present invention will be described by way of examples with reference to the drawings. In the following drawings, in order to make the configuration of the invention easy to understand, a perspective view is partially used, a thick line is used, and the scale of each configuration is appropriately changed.
EXAMPLE 1
(29) Example 1 will be described with reference to
(30) First, hexaborides of rare earth metals and alkaline earth metals are used as materials for field emission electron sources. Specifically, lanthanoid elements such as La, Ce, Pr, Nd, Sm, Eu, Gd, and the like, alkaline earth metals such as Ca, Sr, Ba, and the like can be used, and the materials for field emission electron sources are represented by chemical formulas of LaB.sub.6, CeB.sub.6, PrB.sub.6, NdB.sub.6, SmB.sub.6, EuB.sub.6, GaB.sub.6, CaB.sub.6, SrB.sub.6, BaB.sub.6, and the like, respectively.
(31) A unit lattice is illustrated in
(32) If these hexaborides are used, for example, by melt (liquid phase) crystal growth using a floating zone method or the like, a large single crystal 105 of several tens of mm in length grown in the (001) plane direction of a crystal habit plane where the diameter is several mm and crystals preferentially grow. When the hexaboride is used in a thermal electron source, the single crystal 105 is cut into tips of several hundred m square and several mm in length by cutting, and the (001) plane is used as an electron emission surface. The crystal structure of the hexaboride is a simple cubic lattice as illustrated in
(33) As a result of investigations by the inventors, it has been found that, when the hexaboride is used as the field emission electron source, it is preferable to use the (013) plane which has a work function lower than the (001) plane and in which high brightness electron emission can be obtained.
(34) First, the crystal axis of the hexaboride single crystal 105 was measured by the X-ray Laue method or the like, and the tip 104 was cut out along the (013) crystal axis by cutting, that is, at an angle of 18.4 to the long axis of the hexaboride single crystal 105. Although a cross-sectional shape of the tip 104 to be cut out is arbitrary, it is preferable to cut out the tip in the shape of a square pole or a circular cylindrical shape. In this example, the tip 104 processed into a square pole with a side of 200 m and a length of 5 mm was cut out.
(35) Subsequently, in the electron source according to this example, a method of manufacturing the metal tube used for joining with the tip 104 will be described. A manufacturing process of a metal tube 112 is illustrated in
(36) First, as illustrated in the upper left diagram of
(37) In this example, as described later, since the tip 104 of the electron source is inserted into the metal tube 112 and then joined, the inner diameter of the metal tube 112 is preferably about 1.1 to 1.5 times the maximum diameter of the tip. If the inner diameter of the metal tube is 1.1 times or more, processing tolerance of the tip 104 is usually about 10% and thus, the number of tips 104 that cannot be inserted into the metal tube 112 increases, and a manufacturing yield of the electron source decreases.
(38) On the other hand, if the inner diameter of the metal tube is 1.5 times or more, a dimensional difference between the tip 104 and the inner diameter of the metal tube 112 becomes too large, and a deformation amount of the metal tube 112 in the process of forming and joining a recess described later is large, and a decrease in an assembly accuracy and a decrease in strength, and an increase in power consumption and a decrease in heating response due to increase of heat capacity depending on a volume increase of the metal tube 112 are caused. Accordingly, in the case of the tip 104 having a side of 200 m (square pole having a maximum diameter of about 282 m), the inner diameter of the metal tube 112 is preferably about 310 to 423 m. In this example, the inner diameter of the metal tube 112 is 400 m.
(39) In this example, as described later, since it is necessary to perform spot welding of a filament to the metal tube 112 and it is necessary to withstand high temperature heating during operation for a long time, the metal tube 112 needs to have sufficient strength. For that reason, the thickness of the metal tube is preferably 100 m or more. On the other hand, when the thickness is too thick, since the heat capacity of the metal tube 112 is increased to cause an increase in heating power and a decrease in heating response of the electron source, the thickness is preferably 200 m or less. In this example, the thickness is 100 m.
(40) Subsequently, a joining method of this example will be described.
(41) First, as illustrated in
(42) By adjusting the length of the guide pin 113, the length by which the hexaboride tip 104 protrudes from the inside of the metal tube 112 can be controlled. For example, in the case of producing the field emission electron source or the Schottky electron source, a protrusion amount of the tip is made longer from 2 to 3 mm in order to grind the hexaboride tip 104 by electrolytic polishing as described later. On the other hand, in the case of manufacturing a thermal electron source, a protrusion amount of about 1 to 2 mm is sufficient.
(43) Subsequently, as illustrated in
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(45) During operation, a positional relationship between the metal tube 112 and the hexaboride tip 104 is confirmed with a stereomicroscope 116, and a rotation axis of the hexaboride tip 104 is appropriately adjusted so that each side surface of the hexaboride tip 104 of a square pole coincides with a stroke direction of the blade 115 of the tool. With this configuration, a plurality of recesses 117 are formed so as to surround the central axis from the outer periphery of the metal tube 112, the bottom of each recess 117 is brought into contact with the outer peripheral surface of the hexaboride tip, and as a result, the hexaboride tip 104 can be automatically aligned with the central axis of the metal tube 112 and fixed.
(46) By using this joining method, the metal tube 112 and the hexaboride tip 104 can be uniformly pressure-welded by the recesses 117 formed in two axes and four directions, and mechanically strong joining can be obtained. Since the projections are brought close to the metal tube 112 with equal strokes from two axes and four directions and the metal tube 112 is crushed from the outer periphery thereof to form the recesses 117, the hexaboride tip 104 of the square pole shape can be automatically aligned with and joined to the central axis of the metal tube 112. Assembling accuracy is improved and thus, optical axis alignment of the electron source is facilitated and the yield is also improved. Since a dotted line portion (lower left view of
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(48) Since the hexaboride tip and the metal tube are joined at points of the recesses 117 deviated in the axial direction and thus, the joining strength is further increased. Also, the hexaboride tip and the metal tube are joined at two points in the axial direction and thus, there is an effect that the tip can be prevented from being inclined at the joining part and accuracy of optical axis alignment can be further enhanced. Although the number of stages is not limited, if there are too many stages, since the metal tube 112 necessary for forming the recesses becomes long and the heat capacity is increased, it is desirable to use about two stages.
(49) Subsequently, as illustrated in
(50) Subsequently, the tip end of the hexaboride tip is sharpened by electrolytic polishing. As illustrated in
(51) Thus, a basic structure of the hexaboride field emission electron source according to this example can be completed.
(52) In the example described above, the hexaboride tip 104 cut into a square pole was used. The hexaboride tip 104 can also be processed into a circular cylindrical shape.
(53) Subsequently, this electron source is introduced into a vacuum device to perform surface activation of the hexaboride field emission electron source. Since an oxide and the like are formed on the surface of the hexaboride tip subjected to electrolytic polishing, it is not possible to obtain electron emission as it is. Therefore, first, a positive high electric field is applied to the surface of the hexaboride tip, oxides and the like are removed by field evaporation to clean the surface.
(54) Furthermore, by performing heat annealing at about 1400 to 1800 K for several minutes, field emission with the (013) plane as an electron emission surface can be obtained.
(55) Four-fold symmetrical bright electron emission is obtained. The dark part in the center of the photograph is the (001) plane, and the bright part is the (013) plane and the crystal plane equivalent thereto.
(56) In this example, the recess 117 of the metal tube 112 such as tantalum or niobium and the hexaboride tip 104 are brought into direct contact and joined. For that reason, when the joined part is heated, an intermetallic compound is formed, which may deteriorate the joined part. However, as a result of investigations by the inventors, it was found that, when being used as a field emission electron source, although it is necessary to heat for several minutes at a high temperature of about 1400 K to 1800 K only at first surface cleaning immediately after producing a tip of the electron source, a low temperature of about 1100 K to 1300 K may be sufficient for a flushing or low temperature annealing treatment to prevent gas adsorption thereafter. For that reason, it was found that reaction of the hexaboride with tantalum, niobium, and the like is slow, the amount of a formed intermetallic compound is very small, and there is no decrease in the joining strength due to heating.
(57) As described above, according to this example, it is possible to provide an electron source which can be used stably for a long time even when a hexaboride is used. It is possible to provide a joining structure optimum for the hexaboride in the field emission electron source and a method of manufacturing the joining structure. It is possible to provide a joining method capable of accurately setting optical axis alignment of a minute tip of hexaboride, and to improve the yield of manufacturing the electron source.
EXAMPLE 2
(58) The electron source according to this example will be described with reference to
(59) In this example, a thermal electron source of hexaboride and a Schottky electron source of hexaboride will be described. When the hexaboride is used as a thermal electron source and the Schottky electron source, an operating temperature needs to be raised to a temperature at which thermal electrons can be emitted, and a temperature at which a Schottky barrier can be formed. For that reason, in the structure of Example 1, there is a concern that reaction between the metal tube 112 of tantalum, niobium or the like and the hexaboride tip 104 proceeds to deteriorate the joined part. Therefore, a structure and method of preventing formation of an intermetallic compound and deterioration of a joined part, by continuous use at a strong joining structure and a high temperature, which are improved from Example 1, are described.
(60) The first is a method of inserting a graphite sheet or a metal foil of rhenium as a reaction barrier sheet 122 between the metal tube 112 and the tip 104 of hexaboride to be joined.
(61) None of the materials react with tantalum, niobium, and hexaboride even at high temperatures and when the materials have a thickness of 25 m, the materials are sufficiently thin and flexible and thus, the materials do not disturb the joining method in manufacturing the electron source according to this example. By this method, by contacting the bottom of each of the plurality of recesses 117 of the metal tube 112 with a graphite sheet or rhenium foil on the outer periphery of the hexaboride tip 104, it is possible to obtain a robust and reliable electron source in which an intermetallic compound is not generated and the hexaboride chip does not fall off even when the electron source is heated for a long time.
(62) The second is a method of filling a reaction barrier material such as glassy carbon, or glassy carbon and boron carbide between the metal tube 112 and the hexaboride tip 104. Specifically, the second method is a method in which furan resin or a mixture of furan resin and boron carbide powder is injected between the metal tube 112 and the hexaboride tip 104, and then the metal tube and the hexaboride tip are joined using the tool illustrated in Example 1, and further fired in vacuum to carbonize the furan resin to obtain a reaction barrier material 123 such as glassy carbon.
(63) When being used as the thermal electron source, sharpening of the hexaboride tip 104 is not necessarily required. When being used as a Schottky electron source, the tip is sharpened by electrolytic polishing as in Example 1. Subsequently, an electron source is introduced into a vacuum device to perform surface activation. When being used as the thermal electron source, the surface of the hexaboride tip is naturally cleaned by heating to the operating temperature. When being used as the Schottky electron source, first, surface cleaning is performed by an electric field evaporation method similarly as Example 1, and then heating is performed at high temperature to form an electron emission surface of the (013) plane. In the case of a Schottky electron source, if heating is continued as it is, Ce is always diffused and supplied from the crystal to the surface, and by applying an electric field E from the outside, it can be used as a Schottky electron source from which thermaly excited electrons are emitted over the Schottky barrier lowered by the external electric field E and mirror image potential. The configuration described in this example, that is, the configuration in which the reaction barrier sheet 122 or the reaction barrier material 123 is provided between the metal tube and the hexaboride tip can also be used in the field emission electron source.
(64) As described above, according to this example, it is possible to provide an electron source which can be used stably for a long time even when a hexaboride is used. It is possible to provide a joining structure optimal for the hexaboride in the thermal electron source or the Schottky electron source and a method of manufacturing the joining structure. It is possible to provide a joining method capable of accurately setting the optical axis alignment of a minute tip of the hexaboride, and to improve the yield of manufacturing the electron source.
EXAMPLE 3
(65) Example 3 will be described with reference to
(66)
(67) As described above, according to this example, it is possible to provide a high-brightness, high-resolution electron beam device using an electron source that can be used stably for a long time even when using a hexaboride.
(68) The present invention is not limited to the examples described above, and includes various modification examples.
(69) For example, a length measurement SEM using the thermal field emission electron source or the Schottky electron source, a simple SEM using a thermal electron source, a transmission electron microscope using the field emission electron source or a thermal electron source, and the like may be included.
(70) The present invention includes the following embodiments.
(71) (1) An electron source including;
(72) a filament made of a metal,
(73) a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery,
(74) a graphite sheet or rhenium foil disposed inside the metal tube, and
(75) a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is in contact with the graphite sheet or rhenium foil disposed at the bottom of each of the plurality of recesses of the metal tube.
(76) (2) An electron source including;
(77) a filament made of a metal,
(78) a metal tube that is fixed to the filament and has a plurality of recesses disposed at least in two axial directions so as to surround a central axis at an outer periphery, and
(79) a columnar hexaboride tip that emits an electron, is disposed so as to protrude from the inside of the metal tube to a side opposite to the filament, and is coated with glassy carbon or a mixture of glassy carbon and boride carbon and in contact with the plurality of recesses of the metal tube.
(80) (3) An electron source assembling method including;
(81) a first process of preparing a columnar hexaboride tip, a metal tube, a guide pin shorter in length than the metal tube, a filament made of metal, and a stem including an electrode pin,
(82) a second process of sequentially inserting the guide pin and the columnar hexaboride tip into the metal tube,
(83) a third process of pressure welding the metal tube with a blade of pressure-welding tool having projections in at least two axial directions so as to surround a central axis at an outer periphery of the metal tube,
(84) a fourth process of attaching the filament to the metal tube on a side where the columnar hexaboride tip does not protrude, and
(85) a fifth process of connecting the filament to the electrode pin of the stem.
(86) (4) In the (3) described above, after the second process, a process of inserting a graphite sheet or rhenium foil between the columnar hexaboride tip and the metal tube is further included.
(87) (5) In the (3) described above, after the second process, a process of injecting glassy carbon or a mixture of glassy carbon and boride carbon between the columnar hexaboride tip and the metal tube is further included.
(88) The examples described above are described in detail to explain the present invention in an easy-to-understand manner, and are not necessarily limited to those having all the configurations described. Some of the configurations of an example may be replaced with configurations of other examples, and the configurations of the other example may be added to the configuration of the example. Other configurations may be added, deleted, or substituted for some of the configurations of each example.
REFERENCE SIGNS LIST
(89) 100: electron source
(90) 101: stem
(91) 102: electrode pin
(92) 103: filament
(93) 104: tip
(94) 105: hexaboride single crystal
(95) 106: metal sheet
(96) 107: electron beam welded-part
(97) 108: semi-seamless tube
(98) 109: die
(99) 110: metal pipe
(100) 111: cutter
(101) 112: metal tube
(102) 113: guide pin
(103) 114: pedestal
(104) 115: blade of pressure-welding tool
(105) 116: stereomicroscope
(106) 117: recess
(107) 118: electrolyte solution
(108) 119: counter electrode
(109) 120: power supply
(110) 121: colorimetric thermometer
(111) 122: reaction barrier sheet
(112) 123: reaction barrier material
(113) 124-1, 124-2: positioning jig
(114) 201: metal atom
(115) 202: boron atom
(116) 211: anode
(117) 215: condenser lens
(118) 216: objective lens
(119) 217: astigmatic correction coil
(120) 218: deflection scanning coil
(121) 219: sample
(122) 220: secondary electron detector
(123) 221: element analyzer
(124) 230: electron beam