WO2015041267A1 - アンチコンタミネーショントラップおよび真空応用装置 - Google Patents
アンチコンタミネーショントラップおよび真空応用装置 Download PDFInfo
- Publication number
- WO2015041267A1 WO2015041267A1 PCT/JP2014/074615 JP2014074615W WO2015041267A1 WO 2015041267 A1 WO2015041267 A1 WO 2015041267A1 JP 2014074615 W JP2014074615 W JP 2014074615W WO 2015041267 A1 WO2015041267 A1 WO 2015041267A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- cooling
- contamination trap
- vacuum application
- application apparatus
- refrigerant
- Prior art date
Links
- 238000011109 contamination Methods 0.000 title claims abstract description 67
- 238000001816 cooling Methods 0.000 claims abstract description 247
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 98
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 49
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 239000002826 coolant Substances 0.000 claims abstract 4
- 239000003507 refrigerant Substances 0.000 claims description 44
- 238000010894 electron beam technology Methods 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 13
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 5
- 230000000994 depressogenic effect Effects 0.000 claims description 5
- 239000010409 thin film Substances 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 2
- 239000004020 conductor Substances 0.000 abstract description 4
- 230000009977 dual effect Effects 0.000 abstract 1
- 238000012545 processing Methods 0.000 description 8
- 238000012986 modification Methods 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000009529 body temperature measurement Methods 0.000 description 6
- 230000003287 optical effect Effects 0.000 description 6
- DDMOUSALMHHKOS-UHFFFAOYSA-N 1,2-dichloro-1,1,2,2-tetrafluoroethane Chemical compound FC(F)(Cl)C(F)(F)Cl DDMOUSALMHHKOS-UHFFFAOYSA-N 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000010586 diagram Methods 0.000 description 3
- 238000010884 ion-beam technique Methods 0.000 description 3
- 230000005587 bubbling Effects 0.000 description 2
- 238000004108 freeze drying Methods 0.000 description 2
- 230000035515 penetration Effects 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- RFCAUADVODFSLZ-UHFFFAOYSA-N 1-Chloro-1,1,2,2,2-pentafluoroethane Chemical compound FC(F)(F)C(F)(F)Cl RFCAUADVODFSLZ-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01J—ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS
- H01J37/00—Discharge tubes with provision for introducing objects or material to be exposed to the discharge, e.g. for the purpose of examination or processing thereof
- H01J37/02—Details
- H01J37/18—Vacuum locks ; Means for obtaining or maintaining the desired pressure within the vessel
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B19/00—Machines, plants or systems, using evaporation of a refrigerant but without recovery of the vapour
- F25B19/005—Machines, plants or systems, using evaporation of a refrigerant but without recovery of the vapour the refrigerant being a liquefied gas
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25B—REFRIGERATION MACHINES, PLANTS OR SYSTEMS; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS
- F25B45/00—Arrangements for charging or discharging refrigerant
-
- 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
- H01J37/16—Vessels; Containers
-
- 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
- H01J37/20—Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
-
- 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
- H01J2237/002—Cooling arrangements
-
- 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
- H01J2237/02—Details
- H01J2237/022—Avoiding or removing foreign or contaminating particles, debris or deposits on sample or tube
-
- 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
- H01J2237/02—Details
- H01J2237/028—Particle traps
-
- 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
- H01J2237/18—Vacuum control means
- H01J2237/182—Obtaining or maintaining desired pressure
-
- 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
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2001—Maintaining constant desired temperature
-
- 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
- H01J2237/20—Positioning, supporting, modifying or maintaining the physical state of objects being observed or treated
- H01J2237/2002—Controlling environment of sample
Definitions
- the present invention relates to a vacuum application apparatus such as a charged particle beam apparatus or a freeze drying apparatus.
- processing and observing while freezing and cooling the sample can cause damage due to moisture-containing samples and electron beam irradiation. It enables processing and observation of easily received materials and the like, and is a widely used technique in fields such as biomaterials and organic materials.
- FIB focused ion beam processing equipment
- JP 2010-257617 A Patent Document 1
- the object of the present invention relates to efficient processing or observation with charged particles while cooling. In particular, in a cooled state of a material that may be affected by thermal damage.
- the present invention relates to processing observation, and also relates to effectively reducing the influence of a sample processing method using charged particles by cooling.
- the present invention fixes a sample piece extracted from a sample by ion beam irradiation. And a rotating mechanism for rotating the sample stage in a desired direction.
- the sample stage can be attached to an ion beam apparatus and a transmission electron microscope apparatus, and is movable to thermally connect the sample stage and a cooling source.
- the present invention relates to a sample holder having a heat transfer material, a sample holder, and a separating material that thermally isolates the heat transfer material from the outside. It is possible to perform processing and observation. Has been described as ".
- Patent Document 2 Another background art is Japanese Patent Laid-Open No. 2000-277045 (Patent Document 2).
- Patent Document 2 “[Problem] In the conventional cryostage, the liquid nitrogen container that is a cooling source and the sample are connected by a heat conductor, and the path must be thermally insulated to prevent heat loss. The structure is more complicated than that of the previous stage, and the liquid nitrogen container further increases the size of the stage.
- a cryostage with a scanning electron microscope equipped with an anti-contamination trap separate liquid nitrogen is used.
- a scanning electron microscope equipped with an anti-contamination trap In a scanning electron microscope equipped with an anti-contamination trap, a sample stage, or a sample holder for fixing the sample stage to the sample stage, Alternatively, touch any part of the sample stage with the anti-contamination trap cooling member. The Rukoto, is described as performing. "The cooling of the sample.
- Patent Document 3 Another background art is Japanese Patent Application Laid-Open No. 2007-53048 (Patent Document 3).
- the present invention is a processing apparatus using a focused charged particle beam that can quickly cool a sample, reduce thermal drift, and improve processing accuracy in view of the above situation.
- a sample to be observed and processed by a focused charged particle beam is miniaturized and only the micro sample is locally cooled, or a sample mounting portion having a structure capable of mitigating thermal drift is used. .
- the inventor of the present application diligently studied to bring the cooling temperature of the anti-contamination trap close to the refrigerant temperature, and as a result, the following knowledge was obtained.
- the cooling unit is cooled through a high thermal conductivity material connected to the inner container by vacuum insulation between the two cooling tanks.
- the present application includes a plurality of means for solving the above-mentioned problems. If an example is given, “a structure that cools the internal cooling unit with a vacuum application device, and a cooling tank that contains a refrigerant for cooling the cooling unit, and It has a cooling pipe from the container to the vicinity of the cooling unit, and the refrigerant is supplied to the tip of the cooling unit.
- a refrigerant liquid nitrogen, dry ice, liquid helium, etc.
- an anti-contamination trap in which a cooling part is arranged inside a vacuum sample chamber of a vacuum application apparatus, an introduction pipe for supplying a refrigerant into the cooling part, and a vaporized refrigerant inside the cooling part. What is provided with the discharge pipe which discharges
- the vacuum application apparatus includes an anti-contamination trap, and a cooling part of the anti-contamination trap is arranged inside the vacuum sample chamber, and the introduction pipe supplies the refrigerant to the inside of the cooling part. And a discharge pipe that discharges the vaporized refrigerant inside the cooling unit.
- a discharge pipe is inserted inside the introduction pipe.
- an adjustment unit that adjusts the position of the introduction pipe is provided.
- the cooling unit is made of a material having a higher thermal conductivity than the introduction pipe.
- the cooling unit is made of oxygen-free copper or aluminum.
- the cooling part is hemispherical, U-shaped with a depressed central part, a shape having a plate-like part on the top and bottom, or a shape having a plate-like part on the bottom.
- the embodiment discloses that the refrigerant is liquid nitrogen.
- the cooling tank includes an inner cooling tank that holds the refrigerant and an outer cooling tank that accommodates the inner cooling tank with the heat shield portion interposed therebetween, and the heat shield portion and the vacuum sample chamber are spatially connected.
- the structure is disclosed.
- the vacuum application apparatus includes a cooling holder that cools the sample with the same kind of refrigerant as that of the anti-contamination trap.
- the vacuum application apparatus is a charged particle beam apparatus in which a sample is disposed between the upper magnetic pole and the outer magnetic pole of the objective lens.
- the vacuum application apparatus is a transmission electron microscope that transmits an electron beam through a thin film sample.
- an anti-contamination trap that cools the cooling unit in the vacuum application apparatus and prevents sample contamination, and has a cooling pipe from the cooling tank for storing the refrigerant for cooling the cooling unit to the cooling unit.
- a refrigerant supplied from the cooling tank to the tip of the cooling unit is disclosed.
- the cooling unit and the cooling pipe are disclosed to use materials having high thermal conductivity such as oxygen-free copper and aluminum.
- a tube for releasing bubbles in the cooling pipe is inserted from the cooling tank to the cooling unit.
- the cooling pipe is inclined so as to become lower from the cooling tank toward the cooling unit.
- the cooling pipes are two small-diameter cooling pipes arranged in the vertical direction from the cooling tank to the cooling unit.
- Fig. 1 shows a conventional anti-contamination trap.
- An anti-contamination trap having a conventional structure includes a cooling tank 1 for storing a refrigerant 2, a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1, an oxygen-free copper rod 6 connected to the cooling tank 1, and a cooling unit 5. It consists of The cooling tank 1 has a structure in which the inside of the double wall is evacuated. When the refrigerant 2 is put into the cooling tank 1, the cooling unit 5 is cooled via the oxygen-free copper rod 6 connected to the cooling tank 1.
- FIG. 2 shows a structural example for reducing the heat loss and the cooling time, which are the above-mentioned problems.
- the anti-contamination trap includes a cooling tank 1 for storing the refrigerant 2, a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1, a cooling pipe 7 connected to the cooling tank 1, and a cooling unit 5.
- a cooling tank 1 for storing the refrigerant 2
- a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1
- a cooling pipe 7 connected to the cooling tank 1
- a cooling unit 5 has been.
- FIG. 3 is a specific example of a method for solving a state in which vaporized nitrogen is difficult to escape as bubbles.
- the anti-contamination trap includes a cooling tank 1 for storing the refrigerant 2, a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1, a cooling pipe 7 connected to the cooling tank 1, a cooling unit 5,
- the vaporized nitrogen escape tube 8 is configured to discharge nitrogen vaporized at the tip of the cooling pipe 7.
- the nitrogen bubbles 10 vaporized at the tip of the cooling pipe 7 are discharged through the vaporized nitrogen escape tube 8.
- the vaporized nitrogen bubbles 10 are discharged through the vaporized nitrogen escape tube 8, whereby liquid nitrogen is filled up to the tip of the cooling pipe 7.
- the cooling unit 5 since liquid nitrogen is introduced to the vicinity of the cooling unit 5, the cooling unit 5 can be cooled to -186 ° C. in about 3 minutes.
- FIG. 8 is a configuration diagram of a scanning electron microscope equipped with the anti-contamination trap according to FIG.
- the scanning electron microscope 101 includes an electron optical column 107 that irradiates an electron beam 103, a control device that adjusts each condition of the electron optical column 107, and secondary electrons emitted from the sample by irradiation of the electron beam 103 on the sample.
- a transmission electron detector that can detect electrons transmitted through the sample may be disposed below the sample.
- the objective lens includes an upper magnetic pole 111 and a lower magnetic pole 112.
- a sample stage 113 is provided on the side surface of the electron optical column 107, and a sample holder 109 holding a sample is disposed between the upper magnetic pole 111 and the lower magnetic pole 112 of the objective lens.
- An anti-contamination trap 110 is provided on another side surface of the electron optical column 107 provided with a sample stage 113 that moves the tip of the sample holder 109 in a desired direction.
- the cooling unit 119 at the tip of the anti-contamination trap 110 is located in the vicinity of the sample between the upper magnetic pole 111 and the lower magnetic pole 112 of the objective lens in the vacuum chamber 116.
- FIG. 9 is a partially enlarged view of a scanning electron microscope equipped with the anti-contamination trap according to FIG.
- the anti-contamination trap 110 includes a cooling tank (an inner cooling tank 123 and an outer cooling tank 125), a cooling tank inlet 120 for putting the refrigerant 114 into the cooling tank, and a flange for connecting the vacuum chamber 116 and the cooling tank. 117, a cooling pipe 121 connected to the cooling tank, a cooling pipe adjustment unit 122 for adjusting the position of the cooling pipe 121, and a cooling unit 119.
- the cooling tank has a double structure of an inner cooling tank 123 that holds the refrigerant and an outer cooling tank 125 that accommodates the inner cooling tank 123 with the heat shield portion 124 interposed therebetween.
- the heat shield portion 124 and the vacuum chamber 116 are connected spaces, and the heat shield portion 124 can be in a vacuum state when the vacuum chamber is evacuated.
- the cooling pipe adjustment unit 122 is configured by, for example, a plurality of screw holes provided at the end of the flange 117 and a plurality of screws fastened there holding the cooling pipe 121 in the flange 117 via a collar. Has been.
- the position of the cooling pipe 121 can be adjusted by adjusting a plurality of screws. Since the inner cooling tank 123 and the cooling pipe 121 are welded, a position shift may occur in the cooling pipe 121 due to welding distortion. However, the cooling pipe adjusting unit 122 may not interfere with the upper magnetic pole 111 and the lower magnetic pole 112.
- the cooling part 119 can be arrange
- the cooling pipe 121 is made of SUS or the like, and a high heat conductive material such as oxygen-free copper or aluminum is used for the cooling part 119 at the tip thereof.
- the cooling unit 119 is hemispherical and has a constant wall thickness. Since the cooling unit 119 has a smaller heat capacity per surface area than the cooling pipe 121, it is cooled in a short time when the refrigerant 114 is supplied.
- the vaporized nitrogen escape tube 126 is inserted up to the cooling unit 119. If the vaporized nitrogen escape tube 126 is made of resin, it may be easily inserted from the cooling tank inlet 120 to the cooling part 119, but the tube may be made of metal piping and welded into the cooling pipe.
- the vaporized nitrogen escape tube 126 is inserted up to the cooling unit 119, the nitrogen bubbles 128 vaporized by the cooling unit 119 are discharged through the vaporized nitrogen escape tube 126. Accordingly, when the refrigerant 114 is supplied from the cooling tank inlet 120 into the inner cooling tank 123, the refrigerant 114 is filled up to the cooling unit 119 through the cooling pipe 121, and the cooling unit 119 is cooled.
- the cooling unit 119 since the refrigerant 114 is present inside the cooling unit 119 made of a high thermal conductivity material, the cooling unit 119 is cooled to near the refrigerant temperature.
- the cooling unit 119 of the present embodiment can be made to have a lower temperature than the cooling holder or the like because of its simple structure. it can. Therefore, the temperature difference between the sample cooled by the cooling holder or the like and the anti-contamination trap 110 can be increased, and frost adhesion to the sample surface can be prevented.
- the sample temperature is small.
- the temperature difference from the anti-contamination trap is large, it is possible to prevent frost from adhering to the sample surface.
- the structure shown in FIG. 4 may be taken as a specific example of a method for solving the state in which vaporized nitrogen is difficult to escape as bubbles.
- the anti-contamination trap includes a cooling tank 1 for storing the refrigerant 2, a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1, a cooling pipe 7 having a gradient connected to the cooling tank 1, and a cooling It consists of part 5.
- the structure shown in FIG. 5 may be taken as a specific example of a method for solving the state in which vaporized nitrogen becomes a bubble 10 and is difficult to escape.
- the anti-contamination trap includes a cooling tank 1 for storing the refrigerant 2, a flange 3 for connecting the vacuum chamber 4 and the cooling tank 1, a small-diameter cooling pipe 9 connected to the cooling tank 1, and a cooling unit 5. It is configured.
- the small diameter cooling pipe 9 is arranged in the vertical direction as shown in FIG. Utilizing this, the vaporized nitrogen bubbles 10 in the small-diameter cooling pipe 9 can be discharged from the upper pipe. Therefore, liquid nitrogen is filled up to the tip of the small diameter cooling pipe 9. Since liquid nitrogen is introduced to the vicinity of the cooling unit 5, the cooling unit 5 can be cooled to a temperature close to the refrigerant temperature in a short time.
- FIG. 10 is an explanatory view showing a first modification of the cooling unit.
- the cooling part 119 has a U shape with a depressed center part, and a tiltable sample holder 109 is arranged in a depressed part of the cooling part 119. Even if the sample holder 109 is tilted, there is little variation in the distance to the cooling unit 119, so that frost can be prevented from adhering to the sample surface even if the sample holder 109 is tilted.
- FIG. 11 is an explanatory diagram showing a second modification of the cooling unit.
- the cooling unit 119 has a plate-like portion on the top and bottom, and the plate-like portion extends to the irradiation region of the electron beam 103. Since both the upper and lower plate-like portions have openings, they do not block the electron beam or the like.
- the sample holder 109 is disposed so as to be sandwiched between upper and lower plate-like portions. Since the upper and lower surfaces of the sample holder 109 are covered with the cooling unit 119, it is possible to strongly prevent frost from adhering to the entire surface of the sample.
- FIG. 12 is an explanatory view showing a third modification of the cooling unit.
- the cooling unit 119 has a shape having a plate-like portion at the lower portion, and the plate-like portion extends to the irradiation region of the electron beam 103. Since an opening is formed in the lower plate-like portion, transmitted electrons transmitted through the sample are not blocked.
- the sample holder 109 is disposed on the plate-like portion. Since the surface opposite to the irradiation surface of the electron beam where frost easily adheres is covered with the cooling unit, it is possible to efficiently prevent frost from adhering to the sample surface.
- FIG. 6 shows the temperature measurement results at the tip of the cooling unit 5 having the conventional structure shown in FIG.
- liquid nitrogen was used as the refrigerant 2 and a K thermocouple was attached to the tip of the cooling unit 5.
- the temperature at the tip of the cooling unit 5 reached ⁇ 150 ° C. in about 60 minutes. In this case, until the tip of the cooling unit 5 is stabilized at a low temperature, there is also vibration due to bubbling in which bubbles are actively generated from the refrigerant, and image observation is impossible.
- FIG. 7 shows the temperature measurement results at the tip of the cooling unit 5 having the structure shown in FIG. Temperature measurement was performed using liquid nitrogen as refrigerant 2 and a K thermocouple attached to the tip of the cooling unit 5. The temperature at the tip of the cooling unit 5 reached -186 ° C in about 3 minutes, realizing rapid cooling. is doing. Vibrations caused by bubbling can be quickly subsided and images can be observed immediately.
- this invention is not limited to the above-mentioned Example, Various modifications are included.
- the above-described embodiments have been described in detail for easy understanding of the present invention, and are not necessarily limited to those having all the configurations described.
- the present invention can be implemented even with an out lens SEM whose objective lens has only an upper magnetic pole, a TEM that does not scan an electron beam, and the like.
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
2 冷媒
3 フランジ
4 真空チャンバー
5 冷却部
6 無酸素銅棒
7 冷却パイプ
8 気化窒素逃しチューブ
9 小径冷却パイプ
10 気泡
101 走査電子顕微鏡(SEM)
102 電子源
103 電子ビーム
104 第1コンデンサレンズ
105 第2コンデンサレンズ
106 偏向コイル
107 電子光学鏡筒
108 2次電子検出器
109 試料ホルダ
110 アンチコンタミネーショントラップ
111 上磁極
112 下磁極
113 試料ステージ
114 冷媒
115 冷却タンク
116 真空チャンバー
117 フランジ
119 冷却部
120 冷却タンク注入口
121 冷却パイプ
122 冷却パイプ調整部
123 内側冷却タンク
124 熱シールド部
125 外側冷却タンク
126 気化窒素逃しチューブ
128 気泡
本明細書で引用した全ての刊行物、特許および特許出願をそのまま参考として本明細書にとり入れるものとする。
Claims (24)
- 真空応用装置の真空試料室の内部にその冷却部が配置されるアンチコンタミネーショントラップであって、
前記冷却部の内部に冷媒を供給する導入管と、前記冷却部の内部の気化冷媒を排出する排出管と、を備えたことを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記導入管の内部に前記排出管が挿入されていることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記導入管の位置を調整する調整部を備えることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記冷却部が、前記導入管より熱伝導率が高い材質で構成されていることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記冷却部が、無酸素銅またはアルミニウムで構成されていることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記冷却部が、半球状、中心部が窪んだU字形状、上下に板状部を有する形状、または下部に板状部を有する形状であることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記冷媒が液体窒素であることを特徴とするアンチコンタミネーショントラップ。 - 請求項1のアンチコンタミネーショントラップであって、
前記冷媒を保持する内側冷却タンクと、当該内側冷却タンクを熱シールド部を挟んで収容する外側冷却タンクとを備え、前記熱シールド部と前記真空試料室が空間的に繋がっている構造であることを特徴とするアンチコンタミネーショントラップ。 - アンチコンタミネーショントラップを備え、その真空試料室の内部に前記アンチコンタミネーショントラップの冷却部が配置されている真空応用装置であって、
前記冷却部の内部に冷媒を供給する導入管と、前記冷却部の内部の気化冷媒を排出する排出管と、を備えたことを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記導入管の内部に前記排出管が挿入されていることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記導入管の位置を調整する調整部を備えることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷却部が、前記導入管より熱伝導率が高い材質で構成されていることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷却部が、無酸素銅またはアルミニウムで構成されていることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷却部が、半球状、中心部が窪んだU字形状、上下に板状部を有する形状、または下部に板状部を有する形状であることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷媒が液体窒素であることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷媒を保持する内側冷却タンクと、当該内側冷却タンクを熱シールド部を挟んで収容する外側冷却タンクとを備え、前記熱シールド部と前記真空試料室が空間的に繋がっている構造であることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
前記冷媒と同一種の冷媒で試料を冷却する冷却ホルダを備えることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
当該真空応用装置が、対物レンズの上磁極と外磁極との間に試料を配置する荷電粒子線装置であることを特徴とする真空応用装置。 - 請求項9の真空応用装置であって、
当該真空応用装置が、薄膜試料に電子ビームを透過させる透過電子顕微鏡であることを特徴とする真空応用装置。 - 真空応用装置で装置内冷却部を冷却し試料のコンタミネーションを防ぐアンチコンタミネーショントラップであって、
冷却部を冷却する冷媒を入れる冷却タンクから冷却部まで冷却パイプを有し、
前記冷却タンクから前記冷却部の先端まで冷媒が供給されることを特徴とするアンチコンタミネーショントラップ。 - 請求項20のアンチコンタミネーショントラップにおいて、
冷却部、冷却パイプは無酸素銅やアルミニウムなどの高熱伝導率の材料を用いることを特徴とするアンチコンタミネーショントラップ。 - 請求項20のアンチコンタミネーショントラップにおいて、
冷却パイプ内の気泡を逃すためのチューブを前記冷却タンクから前記冷却部まで挿入することを特徴とするアンチコンタミネーショントラップ。 - 請求項20のアンチコンタミネーショントラップにおいて、
前記冷却パイプは、前記冷却タンクから前記冷却部に向けて低くなるように勾配がつけられていることを特徴とするアンチコンタミネーショントラップ。 - 請求項20のアンチコンタミネーショントラップにおいて、
前記冷却パイプは、前記冷却タンクから前記冷却部まで、上下方向に配置された2本の小径冷却パイプであることを特徴とするアンチコンタミネーショントラップ。
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201480045594.6A CN105474348B (zh) | 2013-09-20 | 2014-09-18 | 防污染阱以及真空应用装置 |
DE112014003582.3T DE112014003582B4 (de) | 2013-09-20 | 2014-09-18 | Kontaminationsverhinderungsfalle und Vakuumanwendungsvorrichtung |
US14/911,960 US10269533B2 (en) | 2013-09-20 | 2014-09-18 | Anti-contamination trap, and vacuum application device |
JP2015537954A JP6172690B2 (ja) | 2013-09-20 | 2014-09-18 | アンチコンタミネーショントラップおよび真空応用装置 |
Applications Claiming Priority (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP2013194807 | 2013-09-20 | ||
JP2013-194807 | 2013-09-20 | ||
JP2014026042 | 2014-02-14 | ||
JP2014-026042 | 2014-02-14 |
Publications (1)
Publication Number | Publication Date |
---|---|
WO2015041267A1 true WO2015041267A1 (ja) | 2015-03-26 |
Family
ID=52688914
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
PCT/JP2014/074615 WO2015041267A1 (ja) | 2013-09-20 | 2014-09-18 | アンチコンタミネーショントラップおよび真空応用装置 |
Country Status (5)
Country | Link |
---|---|
US (1) | US10269533B2 (ja) |
JP (1) | JP6172690B2 (ja) |
CN (1) | CN105474348B (ja) |
DE (1) | DE112014003582B4 (ja) |
WO (1) | WO2015041267A1 (ja) |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2017098574A1 (ja) * | 2015-12-08 | 2017-06-15 | 株式会社日立ハイテクノロジーズ | アンチコンタミネーショントラップおよびその制御方法、ならびに荷電粒子線装置 |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106440481A (zh) * | 2016-11-30 | 2017-02-22 | 无锡溥汇机械科技有限公司 | 一种超声喷雾制冷装置 |
RU2019120098A (ru) | 2016-12-29 | 2021-01-29 | Айпиджи Фотоникс Корпорэйшн | Высокотемпературная оптическая молекулярная геттерная система, предохраняющая от загрязнений |
EP4032648A1 (en) * | 2021-01-25 | 2022-07-27 | Infineon Technologies AG | Arrangement for forming a connection |
Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS543594A (en) * | 1977-06-10 | 1979-01-11 | Hitachi Ltd | Solid surface element analyzer |
JPH04363853A (ja) * | 1991-06-07 | 1992-12-16 | Tel Varian Ltd | イオン注入装置の冷却機構 |
JPH09120789A (ja) * | 1995-10-25 | 1997-05-06 | Jeol Ltd | 試料冷却システム |
JP2000046452A (ja) * | 1998-07-31 | 2000-02-18 | Hitachi Ltd | 低温容器 |
JP2000133188A (ja) * | 1998-10-21 | 2000-05-12 | Hitachi Ltd | 電子顕微鏡の試料冷却ホルダー |
JP2007080698A (ja) * | 2005-09-15 | 2007-03-29 | Fuji Electric Holdings Co Ltd | 試料分析装置 |
JP2009245907A (ja) * | 2008-04-01 | 2009-10-22 | Hitachi High-Technologies Corp | 荷電粒子線装置 |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
NL108507C (ja) * | 1958-09-13 | |||
US3736937A (en) * | 1972-06-08 | 1973-06-05 | Hughes Aircraft Co | Cryogenic tool |
JPS5748274Y2 (ja) * | 1977-07-11 | 1982-10-22 | ||
EP0155700B1 (en) * | 1984-03-22 | 1990-01-31 | Nippon Telegraph And Telephone Corporation | Apparatus for quantitative secondary ion mass spectrometry |
US4833330A (en) * | 1987-11-03 | 1989-05-23 | Gatan Inc. | Anticontaminator for transmission electron microscopes |
US4950901A (en) | 1989-11-06 | 1990-08-21 | Gatan, Incorporated | Specimen cooling holder for side entry transmission electron microscopes |
US6046457A (en) * | 1998-01-09 | 2000-04-04 | International Business Machines Corporation | Charged particle beam apparatus having anticontamination means |
JP2000277045A (ja) | 1999-03-24 | 2000-10-06 | Hitachi Ltd | 走査電子顕微鏡 |
DE10344492B4 (de) | 2003-09-24 | 2006-09-07 | Carl Zeiss Nts Gmbh | Teilchenstrahlgerät |
JP5246995B2 (ja) | 2005-08-19 | 2013-07-24 | 株式会社日立ハイテクサイエンス | 集束荷電粒子ビーム装置 |
JP4598093B2 (ja) * | 2008-02-15 | 2010-12-15 | 株式会社日立ハイテクノロジーズ | 不良検査装置 |
JP5250470B2 (ja) | 2009-04-22 | 2013-07-31 | 株式会社日立ハイテクノロジーズ | 試料ホールダ,該試料ホールダの使用法、及び荷電粒子装置 |
JP5400916B2 (ja) | 2012-03-19 | 2014-01-29 | 本田技研工業株式会社 | 変速機のシンクロ装置 |
JP2014026042A (ja) | 2012-07-25 | 2014-02-06 | Japan Display Inc | 表示装置 |
-
2014
- 2014-09-18 JP JP2015537954A patent/JP6172690B2/ja active Active
- 2014-09-18 US US14/911,960 patent/US10269533B2/en active Active
- 2014-09-18 WO PCT/JP2014/074615 patent/WO2015041267A1/ja active Application Filing
- 2014-09-18 CN CN201480045594.6A patent/CN105474348B/zh active Active
- 2014-09-18 DE DE112014003582.3T patent/DE112014003582B4/de active Active
Patent Citations (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPS543594A (en) * | 1977-06-10 | 1979-01-11 | Hitachi Ltd | Solid surface element analyzer |
JPH04363853A (ja) * | 1991-06-07 | 1992-12-16 | Tel Varian Ltd | イオン注入装置の冷却機構 |
JPH09120789A (ja) * | 1995-10-25 | 1997-05-06 | Jeol Ltd | 試料冷却システム |
JP2000046452A (ja) * | 1998-07-31 | 2000-02-18 | Hitachi Ltd | 低温容器 |
JP2000133188A (ja) * | 1998-10-21 | 2000-05-12 | Hitachi Ltd | 電子顕微鏡の試料冷却ホルダー |
JP2007080698A (ja) * | 2005-09-15 | 2007-03-29 | Fuji Electric Holdings Co Ltd | 試料分析装置 |
JP2009245907A (ja) * | 2008-04-01 | 2009-10-22 | Hitachi High-Technologies Corp | 荷電粒子線装置 |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2017098574A1 (ja) * | 2015-12-08 | 2017-06-15 | 株式会社日立ハイテクノロジーズ | アンチコンタミネーショントラップおよびその制御方法、ならびに荷電粒子線装置 |
WO2017098958A1 (ja) * | 2015-12-08 | 2017-06-15 | 株式会社日立ハイテクノロジーズ | 荷電粒子線装置およびその制御方法 |
DE112016004864T5 (de) | 2015-12-08 | 2018-07-19 | Hitachi High-Technologies Corporation | Vorrichtung mit einem Strahl geladener Partikel und Steuerungsverfahren dafür |
CN108885962A (zh) * | 2015-12-08 | 2018-11-23 | 株式会社日立高新技术 | 带电粒子束装置及其控制方法 |
US10784074B2 (en) | 2015-12-08 | 2020-09-22 | Hitachi High-Technologies Corporation | Charged particle beam apparatus and control method thereof |
DE112016004864B4 (de) | 2015-12-08 | 2021-12-30 | Hitachi High-Tech Corporation | Vorrichtung mit einem Strahl geladener Partikel und Steuerungsverfahren dafür |
Also Published As
Publication number | Publication date |
---|---|
JP6172690B2 (ja) | 2017-08-02 |
US10269533B2 (en) | 2019-04-23 |
US20160203940A1 (en) | 2016-07-14 |
DE112014003582B4 (de) | 2020-08-06 |
DE112014003582T5 (de) | 2016-05-04 |
CN105474348B (zh) | 2018-02-23 |
JPWO2015041267A1 (ja) | 2017-03-02 |
CN105474348A (zh) | 2016-04-06 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
JP6093752B2 (ja) | イオンビーム装置 | |
US8779380B2 (en) | Ion beam device | |
JP6172690B2 (ja) | アンチコンタミネーショントラップおよび真空応用装置 | |
WO2018025849A1 (ja) | 荷電粒子線装置及び走査電子顕微鏡 | |
JP6286609B1 (ja) | 荷電粒子顕微鏡内での低温試料処理 | |
US9543112B2 (en) | Specimen cryo holder and dewar | |
JP5039274B2 (ja) | 粒子放射装置 | |
JP5914578B2 (ja) | 凍結含水試料をマイクロプローブへ結合する方法 | |
JP5560033B2 (ja) | 冷却試料ホールダ及び試料の冷却加工方法 | |
US9916963B2 (en) | Specimen loading method, specimen stage, and charged particle beam device | |
JP6584787B2 (ja) | プラズマイオン源および荷電粒子ビーム装置 | |
EP3113208B1 (en) | Electron microscope | |
EP3477679A1 (en) | Improved cryogenic cell for mounting a specimen in a charged particle microscope | |
CN108885962B (zh) | 带电粒子束装置及其控制方法 | |
JP2017016810A (ja) | 荷電粒子線装置、および試料ホルダの温度制御方法 | |
JP7382299B2 (ja) | 荷電粒子線装置 | |
JP5216389B2 (ja) | 荷電粒子線装置 | |
JP2024017051A (ja) | 試料ホルダーおよび荷電粒子線装置 | |
JP2023026841A (ja) | 試料ホルダーおよび荷電粒子線装置 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
WWE | Wipo information: entry into national phase |
Ref document number: 201480045594.6 Country of ref document: CN |
|
121 | Ep: the epo has been informed by wipo that ep was designated in this application |
Ref document number: 14846231 Country of ref document: EP Kind code of ref document: A1 |
|
ENP | Entry into the national phase |
Ref document number: 2015537954 Country of ref document: JP Kind code of ref document: A |
|
WWE | Wipo information: entry into national phase |
Ref document number: 14911960 Country of ref document: US |
|
WWE | Wipo information: entry into national phase |
Ref document number: 112014003582 Country of ref document: DE |
|
122 | Ep: pct application non-entry in european phase |
Ref document number: 14846231 Country of ref document: EP Kind code of ref document: A1 |