FR2477769A1 - Sample treatment chamber for electron microscope - has sealed vertical passage traversed by pair of high tension electrodes overlying sample carrier for in situ treatment - Google Patents
Sample treatment chamber for electron microscope - has sealed vertical passage traversed by pair of high tension electrodes overlying sample carrier for in situ treatment Download PDFInfo
- Publication number
- FR2477769A1 FR2477769A1 FR8005037A FR8005037A FR2477769A1 FR 2477769 A1 FR2477769 A1 FR 2477769A1 FR 8005037 A FR8005037 A FR 8005037A FR 8005037 A FR8005037 A FR 8005037A FR 2477769 A1 FR2477769 A1 FR 2477769A1
- Authority
- FR
- France
- Prior art keywords
- sample
- treatment
- electron microscope
- microscope
- sample carrier
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 6
- 238000004458 analytical method Methods 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 4
- 230000008021 deposition Effects 0.000 abstract description 2
- 239000004020 conductor Substances 0.000 abstract 1
- 238000009413 insulation Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000010849 ion bombardment Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 230000037452 priming Effects 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000000992 sputter etching Methods 0.000 description 1
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
- H01J37/26—Electron or ion microscopes; Electron or ion diffraction tubes
- H01J37/261—Details
-
- 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
-
- 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
- H01J37/30—Electron-beam or ion-beam tubes for localised treatment of objects
- H01J37/305—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching
- H01J37/3053—Electron-beam or ion-beam tubes for localised treatment of objects for casting, melting, evaporating, or etching for evaporating or etching
Landscapes
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Physics & Mathematics (AREA)
- Engineering & Computer Science (AREA)
- Plasma & Fusion (AREA)
- Analysing Materials By The Use Of Radiation (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
Description
La présente invention a pour objet un dispositif pour microscope électronique permettant un traitement in situ d'échantillons. Elle trouve une application en instrumentation scientifique et notamment en microscopie électronique à balayage. The present invention relates to a device for an electronic microscope allowing in situ processing of samples. It finds an application in scientific instrumentation and in particular in scanning electron microscopy.
L'observation au microscope à balayage nécessite un traitement préalable de la surface des échantillons, consistant, soit en une pulvérisation cathodique, soit en un dépôt de couche mince conductrice. Observation using a scanning microscope requires prior treatment of the surface of the samples, consisting either of sputtering or of a deposit of a thin conductive layer.
Dans l'art antérieur, ce traitement est effectué dans une enceinte spéciale située à l'extérieur de la chambre du microscope. Cette technique présente l'inconvénient entraîner un risque de pollution des échantillons lors de leur transfert de l'enceinte de traitement à la chambre du microscope.In the prior art, this treatment is carried out in a special enclosure situated outside the microscope chamber. This technique has the disadvantage of causing a risk of pollution of the samples during their transfer from the treatment chamber to the microscope chamber.
La présente invention a justement pour objet un dispositif destiné à éviter cet inconvénient. The object of the present invention is precisely a device intended to avoid this drawback.
La difficulté essentielle posée par la réalisation d'un dispositif de traitement d'échantillons tient à la nécessité de satisfaire simultanément à deux conditions expérimentales difficilement conciliables - obtention d'une décharge électrique sous vide partiel
(en atmosphère neutre ou réactive), - possibilité d'introduire les échantillons dans la
chambre du microscope sitôt après traitement acec un
minimum de manipulation et sans risque de contamina
tion par l'atmosphère.The essential difficulty posed by the realization of a device for processing samples stems from the need to simultaneously satisfy two experimental conditions which are difficult to reconcile - obtaining an electric discharge under partial vacuum.
(in a neutral or reactive atmosphere), - possibility of introducing the samples into the
microscope chamber immediately after treatment with a
minimum handling and no risk of contamination
tion by atmosphere.
Manifestement, la solution employée dans l'art antérieur, qui consiste à effectuer le traitement préalable dans une enceinte extérieure au microscope, ne répond pas à ces exigences. Le dispositif de 1 'in- vention y parvient grâce aux caractéristiques suivantes : il comprend, montée sur le sas du microscope, une bride munie d'un passage étanche haute tension traversé par deux électrodes reliées à une source haute tension. Obviously, the solution used in the prior art, which consists in carrying out the preliminary treatment in an enclosure external to the microscope, does not meet these requirements. The device of the invention achieves this by virtue of the following characteristics: it comprises, mounted on the airlock of the microscope, a flange provided with a high voltage sealed passage crossed by two electrodes connected to a high voltage source.
Cet ensemble constitue une antichambre de traitement dans laquelle les échantillons peuvent être amenés à l'aide de la canne même de manutention du microscope.This assembly constitutes a processing anteroom into which the samples can be brought using the same rod for handling the microscope.
Après traitement, les échantillons sont poussés dans la chambre d'analyse du microscope sans remise à l'air. After treatment, the samples are pushed into the analysis chamber of the microscope without return to the air.
De toute façon, les caractéristiques et avantages de l'invention apparaîtront mieux après la description qui suit d'un exemple de réalisation donné à titre explicatif et nullement limitatif. Cette description se réfère à des dessins sur lesquels
- la figure 1 représente une coupe transversale d'un dispositif selon l'invention,
- la figure 2 représente une coupe longitudinale de ce même dispositif.In any case, the characteristics and advantages of the invention will appear better after the following description of an exemplary embodiment given by way of explanation and in no way limiting. This description refers to drawings in which
FIG. 1 represents a cross section of a device according to the invention,
- Figure 2 shows a longitudinal section of the same device.
Le dispositif représenté sur les figures 1 et 2 comprend une chambre d'analyse 8 de microscope électronique à balayage, un sas d'introduction comportant une partie 10 solidaire de ladite chambre et une partie amovible 10', une bride rallonge 11 disposée entre les parties 10 et 10', cette bride étant reliée à un appendice 12 muni d'un passage étanche 13 traversé par deux électrodes 14 entourées d'une gaine isolante 16 (par exemple en céramique), ces électrodes étant reliées à une source haute tension 18. Un porte-échantillons 20 relié à une canne de manutention 22 permet d'amener les échantillons 24, d'abord sous les électrodes 14 pour le traitement désiré, puis dans la chambre 8. L'ensemble se complète par une entrée de gaz 26 et une jauge de pression 28. The device shown in FIGS. 1 and 2 comprises an analysis chamber 8 of a scanning electron microscope, an introductory airlock comprising a part 10 integral with said chamber and a removable part 10 ′, an extension flange 11 disposed between the parts 10 and 10 ′, this flange being connected to an appendage 12 provided with a sealed passage 13 crossed by two electrodes 14 surrounded by an insulating sheath 16 (for example made of ceramic), these electrodes being connected to a high voltage source 18. A sample holder 20 connected to a handling rod 22 makes it possible to bring the samples 24, first under the electrodes 14 for the desired treatment, then in the chamber 8. The assembly is completed by a gas inlet 26 and a pressure gauge 28.
La disposition décrite permet - de ne pas nécessiter de modification importante du
sas d'introduction des échantillons puisque les orga
nes supplémentaires prennent place entre les deux
parties séparables 10 et 10' ; - un montage et un démontage rapides du dispositif (par
une fixation à balonnette par exemple) I - une bonne maniabilité des moyens de réglage de la
position des échantillons, puisque la platine gonio
métrique du microscope peut être utilisée - d'utiliser des composants standard dans la technique
du vide (passages électriques, arrivées de gaz, jau
ge, etc...).The arrangement described makes it possible - not to require any significant modification of the
airlock for introducing samples since the organ
nes take place between the two
separable parts 10 and 10 '; - rapid assembly and disassembly of the device (by
a bar attachment for example) I - good handling of the means for adjusting the
position of the samples, since the gonio stage
metric of the microscope can be used - to use standard components in the technique
vacuum (electrical passages, gas inlets, gauge
ge, etc ...).
A titre explicatif, il peut être indiqué que le dispositif de l'invention peut être utilisé avec une alimentation haute tension continue 0-1000 V/100 mA dont les sorties sont à un potentiel non défini par rapport à la masse. De cette manière, en modifiant les potentiels respectifs des électrodes par rapport à l'échantillon en cours de traitement, plusieurs types d'opérations peuvent être réalisés
i) nettoyage de la surface par bombardement,
ii) décapage ionique, iii) dépôt d'une couche mince conductrice.By way of explanation, it may be indicated that the device of the invention can be used with a direct high voltage supply 0-1000 V / 100 mA whose outputs are at a potential not defined with respect to ground. In this way, by modifying the respective potentials of the electrodes relative to the sample being processed, several types of operations can be carried out.
i) surface cleaning by bombardment,
ii) ion etching, iii) deposition of a thin conductive layer.
Dans les trois cas, l'échantillon est mis à la masse par l'intermédiaire de la canne d'introduction du sas. In all three cases, the sample is earthed via the airlock introduction rod.
Le nettoyage de la surface est effectué par bombardement ionique (d'ions Ar+ en général) de faible énergie cinétique (4 à 5 eV). The cleaning of the surface is carried out by ion bombardment (of Ar + ions in general) with low kinetic energy (4 to 5 eV).
Pour un décapage ionique, un bombardement d'ions énergétiques (0,3 à 1 keV) est obtenu en fixant le potentiel d'une des électrodes par rapport à la masse grâce à un potentiomètre placé entre les deux pôles de l'alimentation haute tension, le point milieu étant relié à la masse. For an ionic stripping, a bombardment of energetic ions (0.3 to 1 keV) is obtained by fixing the potential of one of the electrodes relative to the ground thanks to a potentiometer placed between the two poles of the high voltage power supply , the midpoint being connected to ground.
Dans tous les cas, le courant ionique est limité à quelques milliampères. L'amorçage du plasma, dans le cas de l'argon, est obtenu pour une pression partielle d'environ 0,2 torr. In all cases, the ion current is limited to a few milliamps. Priming of the plasma, in the case of argon, is obtained for a partial pressure of approximately 0.2 torr.
Le dispositif de l'invention permet : - la suppression du ncarré noir" de contamination ob
servé en image d'électrons secondaires avec les tech
niques antérieures, - l'amélioration des contrastes en image d'électrons
secondaires.The device of the invention allows: - the elimination of the black ncarré "of contamination ob
served as an image of secondary electrons with tech
previous nics, - the improvement of contrasts in electron image
secondary.
On peut également citer, comme autres possibilités du dispositif de l'invention, l'abrasion ionique in situ. Le dispositif décrit permet, par décapages successifs et sans démontage de l'échantillon, d'analyser le profil d'un défaut depuis son,point d'émergence à la surface jusqu'à son extrémité dans le -volume de l'échantillon. Mention may also be made, as other possibilities of the device of the invention, of ionic abrasion in situ. The device described makes it possible, by successive stripping and without dismantling the sample, to analyze the profile of a defect from its, point of emergence at the surface to its end in the volume of the sample.
Claims (3)
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8005037A FR2477769A1 (en) | 1980-03-06 | 1980-03-06 | Sample treatment chamber for electron microscope - has sealed vertical passage traversed by pair of high tension electrodes overlying sample carrier for in situ treatment |
| JP2893581U JPS579159U (en) | 1980-03-06 | 1981-03-02 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| FR8005037A FR2477769A1 (en) | 1980-03-06 | 1980-03-06 | Sample treatment chamber for electron microscope - has sealed vertical passage traversed by pair of high tension electrodes overlying sample carrier for in situ treatment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| FR2477769A1 true FR2477769A1 (en) | 1981-09-11 |
| FR2477769B1 FR2477769B1 (en) | 1982-09-24 |
Family
ID=9239385
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| FR8005037A Granted FR2477769A1 (en) | 1980-03-06 | 1980-03-06 | Sample treatment chamber for electron microscope - has sealed vertical passage traversed by pair of high tension electrodes overlying sample carrier for in situ treatment |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JPS579159U (en) |
| FR (1) | FR2477769A1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0369913A1 (en) * | 1988-11-18 | 1990-05-23 | CHAIXMECA, Sàrl | Device for the transfer and atmospherically controlled reactions in situ of samples to be examined in transmission electron microscopy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3858049A (en) * | 1973-09-17 | 1974-12-31 | Etec Corp | Method and apparatus for sem specimen coating and transfer |
| DE2511449A1 (en) * | 1975-03-15 | 1976-09-16 | Leybold Heraeus Gmbh & Co Kg | Sample charging valve for high vacuum systems - having graphite boxes around sample support rod sealed to valve using O rings |
-
1980
- 1980-03-06 FR FR8005037A patent/FR2477769A1/en active Granted
-
1981
- 1981-03-02 JP JP2893581U patent/JPS579159U/ja active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3858049A (en) * | 1973-09-17 | 1974-12-31 | Etec Corp | Method and apparatus for sem specimen coating and transfer |
| DE2511449A1 (en) * | 1975-03-15 | 1976-09-16 | Leybold Heraeus Gmbh & Co Kg | Sample charging valve for high vacuum systems - having graphite boxes around sample support rod sealed to valve using O rings |
Non-Patent Citations (1)
| Title |
|---|
| EXRV/76 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0369913A1 (en) * | 1988-11-18 | 1990-05-23 | CHAIXMECA, Sàrl | Device for the transfer and atmospherically controlled reactions in situ of samples to be examined in transmission electron microscopy |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2477769B1 (en) | 1982-09-24 |
| JPS579159U (en) | 1982-01-18 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| ST | Notification of lapse |