# US 8,785,883 B2 · Transmission electron microscope, and method of observing specimen

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- Number: US 8,785,883 B2
- Document ID: US8785883B2
- Status: Granted
- Kind: B2
- Application number: 12/918,619
- Filed: 2009-04-27
- Published: 2011-03-10
- Granted: 2014-07-22
- Earliest claimed: 2008-04-28
- Assignees: Hitachi High-Technologies Corporation
- Applicants: Eiko Nakazawa; Hiroyuki Kobayashi; Susumu Kuwabata
- Inventors: Eiko Nakazawa; Hiroyuki Kobayashi; Susumu Kuwabata
- Web page: https://patentgrep.com/patent/US8785883B2

## CPC

- H01J 37/20: Means for supporting or positioning the object or the material; Means for adjusting diaphragms or lenses associated with the support
- G01N 23/04: and forming images of the material
- G01N 23/2251: using incident electron beams, e.g. scanning electron microscopy [SEM]
- H01J 37/26: Electron or ion microscopes; Electron or ion diffraction tubes
- H01J 37/261: {Details}
- G01N 1/2813: {Producing thin layers of samples on a substrate, e.g. smearing, spinning-on (G01N1/30 takes precedence)}
- G01N 2001/4027: {evaporation leaving a concentrated sample}
- H01J 37/3007: {Electron or ion-optical systems}
- H01J 2237/2002: Controlling environment of sample
- H01J 2237/20214: Rotation
- H01J 2237/204: Means for introducing and/or outputting objects
- H01J 2237/206: Modifying objects while observing
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

Provided is means which enables observation of the shape of a specimen as it is without deforming the specimen. Observation is made by allowing a specimen-holding member having an opening (for example, microgrid and mesh) to hold an ionic liquid and charging a specimen thereto, to allow the specimen to suspend in the ionic liquid. Furthermore, in the proximity of the specimen-holding member, a mechanism of injecting an ionic liquid (ionic liquid introduction mechanism) and/or an electrode are provided. When a voltage is applied to the electrode, the specimen moves or deforms in the ionic liquid. How the specimen moves or deforms can be observed. Furthermore, in the proximity of specimen-holding member, an evaporation apparatus is provided to enable charge of the specimen into the ionic liquid while evaporating. Furthermore, in the proximity of the specimen-holding member, a microcapillary is provided to charge a liquid-state specimen into the ionic liquid. Note that the specimen-holding member is designed to be rotatable.

## Claims

### Claim 1

A transmission electron microscope in which an electron beam is applied to a specimen set in a specimen chamber and an image of the specimen is formed from the electron beam transmitted through the specimen, the transmission electron microscope comprising:
a specimen holder for introducing the specimen into the specimen chamber, wherein the specimen holder has a specimen-holding member at a tip portion, and the specimen-holding member has an opening for transmitting the electron beam and for holding, entirely by surface tension, an ionic liquid having the specimen charged therein, wherein the ionic liquid fills the entire opening, and
an image forming unit for forming an image of the specimen based on the electron beam transmitted through the specimen.

### Claim 2 (depends on 1)

The transmission electron microscope according to claim 1, further comprising a liquid introduction mechanism for introducing the ionic liquid into the opening of the specimen-holding member.

### Claim 3 (depends on 2)

The transmission electron microscope according to claim 2, further comprising a liquid introduction-amount controlling unit for controlling an introduction amount of the ionic liquid.

### Claim 4 (depends on 1)

The transmission electron microscope according to claim 1, further comprising voltage application means which applies a voltage to the specimen in the ionic liquid held in the opening of the specimen-holding member.

### Claim 5 (depends on 1)

The transmission electron microscope according to claim 1, further comprising specimen evaporation means which evaporates the specimen by heating and charges the specimen in the ionic liquid.

### Claim 6 (depends on 1)

The transmission electron microscope according to claim 1, further comprising a liquid introduction mechanism for independently introducing any one of a liquid-state specimen, a solution containing a powder specimen dissolved therein, or a reagent specimen solution, and the ionic liquid.

### Claim 7 (depends on 1)

The transmission electron microscope according to claim 1, further comprising a specimen-holding member driving mechanism for rotating the specimen-holding member.

### Claim 8

A method for observing a specimen in which an electron beam is applied to a specimen set in a specimen chamber and a specimen image formed from the electron beam transmitted through the specimen is observed, the method comprising:
a step of introducing an ionic liquid having the specimen dispersed therein into an opening of a specimen-holding member at a tip potion of a specimen holder for introducing the specimen to the specimen chamber, wherein the ionic liquid is held in the opening entirely by surface tension, and the ionic liquid fills the entire opening,
a step of applying the electron beam to the ionic liquid, and
a step of observing a specimen image formed based on the electron beam transmitted through the specimen.

### Claim 9 (depends on 8)

The method for observing a specimen according to claim 8, wherein, in the step of introducing the ionic liquid, the specimen holder is set in the specimen chamber, and thereafter, the ionic liquid is introduced in the opening of the specimen-holding member by use of a liquid introduction mechanism.

### Claim 10 (depends on 9)

The method for observing a specimen according to claim 9, wherein an ionic liquid introduction amount is controlled by a liquid introduction-amount controlling unit.

### Claim 11 (depends on 8)

The method for observing a specimen according to claim 8, further comprising the step of applying a voltage to the specimen in the ionic liquid contained in the opening of the specimen-holding member.

### Claim 12 (depends on 8)

The method for observing a specimen according to claim 8, wherein, in the step of introducing the ionic liquid, the ionic liquid is introduced into the specimen-holding member and subsequently the specimen is evaporated by heating and charged into the ionic liquid.

### Claim 13 (depends on 8)

The method for observing a specimen according to claim 8, wherein, in the step of introducing the ionic liquid, the specimen holder is set in the specimen chamber, and thereafter, any one of a liquid-state specimen, a solution containing a powder specimen dissolved therein, or a reagent specimen solution, and the ionic liquid are independently introduced in the opening of the specimen-holding member by use of the liquid introduction mechanism.

### Claim 14 (depends on 8)

The method for observing a specimen according to claim 8, wherein, in the step of applying the electron beam, the electron beam is applied to the specimen while the specimen-holding member is rotated by use of a specimen-holding member driving mechanism.

### Claim 15 (depends on 1)

The transmission electron microscope according to claim 1, wherein the specimen-holding member comprises a thin film, and the opening is formed in the thin film.

### Claim 16 (depends on 8)

The method for observing a specimen according to claim 8, wherein the specimen-holding member comprises a thin film, and the opening is formed in the thin film.
