DE19729526C2 - Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures - Google Patents

Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures

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Publication number
DE19729526C2
DE19729526C2 DE1997129526 DE19729526A DE19729526C2 DE 19729526 C2 DE19729526 C2 DE 19729526C2 DE 1997129526 DE1997129526 DE 1997129526 DE 19729526 A DE19729526 A DE 19729526A DE 19729526 C2 DE19729526 C2 DE 19729526C2
Authority
DE
Germany
Prior art keywords
sample table
scanning electron
high temperatures
electron microscopes
situ imaging
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.)
Expired - Fee Related
Application number
DE1997129526
Other languages
German (de)
Other versions
DE19729526A1 (en
Inventor
Frank Siegelin
Hans-Joachim Dr Kleebe
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
KLEEBE HANS JOACHIM DR
Original Assignee
KLEEBE HANS JOACHIM DR
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by KLEEBE HANS JOACHIM DR filed Critical KLEEBE HANS JOACHIM DR
Priority to DE1997129526 priority Critical patent/DE19729526C2/en
Publication of DE19729526A1 publication Critical patent/DE19729526A1/en
Application granted granted Critical
Publication of DE19729526C2 publication Critical patent/DE19729526C2/en
Anticipated expiration legal-status Critical
Expired - Fee Related legal-status Critical Current

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
    • G01N23/225—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material using electron or ion
    • 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
    • H01J37/244—Detectors; Associated components or circuits therefor
    • 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
    • H01J2237/244—Detection characterized by the detecting means
    • H01J2237/2443—Scintillation detectors

Description

Die Erfindung betrifft einen beheizbaren Probentisch zur in-situ Abbildung in Rasterelektronenmikroskopen bei hohen Temperaturen nach dem Oberbegriff des Anspruchs 1.The invention relates to a heatable sample table for in-situ imaging in Scanning electron microscopes at high temperatures according to the generic term of Claim 1.

Mit den bisher verfügbaren Geräten ist es möglich, Proben im Rasterelektronenmikroskop bis auf Temperaturen von ca. 1500°C aufzuheizen, wobei von in-situ Abbildungen, speziell in Mikroskopen mit Everheart-Thornley-Detektor, jedoch nur bis zu Temperaturen von ca. 1100°C berichtet wurden. Diese Beschränkung ist vor allem für materialwissenschaftliche Fragestellungen problematisch, da viele interessante Prozesse erst im Temperaturbereich oberhalb 1200°C beginnen (DE-AS 11 31 820; DE 17 35 700 A1).With the devices available so far, it is possible to take samples in a scanning electron microscope heat up to temperatures of approx. 1500 ° C, using in-situ images, especially in microscopes with Everheart-Thornley detector, but only up to Temperatures of around 1100 ° C have been reported. This limitation is mostly for Material science issues problematic because of many interesting processes begin only in the temperature range above 1200 ° C (DE-AS 11 31 820; DE 17 35 700 A1).

Ein weiterer Nachteil der bisher bekannten Geräte ist deren relativ komplexe Bauform. Hierdurch werden sowohl Einbau und Wechsel der Proben erschwert, als auch die Kosten für Herstellung und Wartung der Vorrichtung erhöht.Another disadvantage of the previously known devices is their relatively complex design. This complicates the installation and replacement of the samples as well as the costs increased for manufacturing and maintenance of the device.

Ziel ist daher die Konstruktion eines beheizbaren Probentisches mit möglichst einfacher Bauform, der in der Lage ist, eine Probentemperatur von 1600°C zu erreichen, so daß gleichzeitig in-situ Abbildungen möglich sind.The aim is therefore to design a heatable sample table that is as simple as possible Design that is able to reach a sample temperature of 1600 ° C, so that at the same time in-situ images are possible.

Dieses Problem wird durch die im Patentanspruch 1 aufgeführten Merkmale gelöst. Eine weitere Ausgestaltung der Erfindung ist dem Anspruch 2 zu entnehmen.This problem is solved by the features listed in claim 1. A A further embodiment of the invention can be found in claim 2.

Durch das paßgenaue Ineinanderstecken des tiegel- und des trichterförmigen Formteils ergibt sich eine vollständige Kapselung der gesamten Heizdrahtanordnung. Dies hat neben der Abschirmung der am Heizleiter entstehenden thermischen Elektronen den weiterem Vorteil, daß ein Abdampfen des Heizleitermaterials in den Probenraum und somit eine Kontamination und Beeinträchtigung der Probe verhindert wird. Nur so lassen sich Abbildungstemperaturen von deutlich über 1200°C erzielen.By fitting the crucible and funnel-shaped molded parts into each other the entire heating wire arrangement is completely encapsulated. This has besides the shielding of the thermal electrons generated on the heating conductor Advantage that evaporation of the heating conductor material in the sample space and thus a  Contamination and impairment of the sample is prevented. This is the only way Achieve imaging temperatures well above 1200 ° C.

Ein weiterer wesentlicher Vorteil des Stecksystems besteht in dessen einfachem Aufbau. Da es sich bei allen Teilen, die dieser hohen Temperatur ausgesetzt sind, um Verschleißteile handelt, ist es wichtig, diese einfach und kostengünstig austauschen zu können. Wie im Ausführungsbeispiel gezeigt, ist auf diese Weise auch die auf dem Probenteller angebrachte Probe leicht zugänglich.Another major advantage of the plug-in system is its simple structure. Since all parts that are exposed to this high temperature are Wear parts, it is important to replace them easily and inexpensively can. As shown in the exemplary embodiment, this is also the one on the Sample plate attached sample easily accessible.

Ein Ausführungsbeispiel der Erfindung ist in der Zeichnung dargestellt und wird im folgenden näher beschrieben.An embodiment of the invention is shown in the drawing and is in following described in more detail.

Es zeigtIt shows

Fig. 1 eine Explosionsdarstellung des Ofens, bestehend aus Tiegel, Heizleiter und Deckel; Figure 1 is an exploded view of the furnace, consisting of a crucible, heat conductor and lid.

Fig. 2 einen Schnitt durch Ofen, Probe und Thermoelement; Fig. 2 is a section through the oven, the sample and the thermocouple;

Die Probe 1 befindet sich auf einem Probenteller 2 aus Graphit, welcher wiederum auf einem Thermoelement 3 befestigt ist, welches auch zur Messung und Regelung der Temperatur verwendet wird. Diese Anordnung ist von einem Ofen umgeben, mit dem die Probe aufgeheizt werden kann. Der Ofen besteht aus drei Teilen. Einem Tiegel 4, einer Heizung 5 und einem Deckel 6, wobei Tiegel 4 und Deckel 6 aus dichtem, hochtemperaturbeständigem Aluminiumoxid gefertigt sind. Der Deckel 6 ist trichterförmig ausgeführt, so daß er zusammen mit dem Tiegel 4 die Heizung 5 vollständig umschließt. Der Tiegel 4 ist mit zwei seitlichen Durchführungen für den Heizdraht 7 und mit einem zentrischen Loch im Boden zur Durchführung des Thermoelements 3 versehen (siehe Fig. 2). Der Heizdraht 7 besteht aus Tantal-Draht, welcher mittels Aluminiumoxid-Röhrchen 8 isoliert ist und wie in Fig. 2 gezeigt, geformt ist. Hierbei ist es günstig mehrere Adern Tantaldraht (ca. 3-6) durch eine gemeinsame Isolierung zu führen.The sample 1 is located on a sample plate 2 made of graphite, which in turn is attached to a thermocouple 3 , which is also used for measuring and controlling the temperature. This arrangement is surrounded by an oven with which the sample can be heated. The oven consists of three parts. A crucible 4 , a heater 5 and a lid 6 , the crucible 4 and lid 6 being made of dense, high-temperature-resistant aluminum oxide. The cover 6 is funnel-shaped so that it completely encloses the heater 5 together with the crucible 4 . The crucible 4 is provided with two lateral passages for the heating wire 7 and with a central hole in the bottom for the passage of the thermocouple 3 (see FIG. 2). The heating wire 7 consists of tantalum wire, which is insulated by means of aluminum oxide tubes 8 and is shaped as shown in FIG. 2. In this case, it is advantageous to route several tantalum wires (approx. 3-6) through a common insulation.

Claims (2)

1. Beheizbarer Probentisch zur in-situ Abbildung in Rasterelektronenmikroskopen bei hohen Temperaturen, wobei die Beheizung mittels eines mit Keramik isolierten Heizdraht erfolgt, dadurch gekennzeichnet, daß der Heizdraht (7) von einem tiegel- und einem trichterförmigen Formteil (4, 6) aus Aluminiumoxid umgeben ist, welche paßgenau ineinander steckbar sind.1. Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures, the heating being carried out by means of a heating wire insulated with ceramic, characterized in that the heating wire ( 7 ) has a crucible and a funnel-shaped molded part ( 4 , 6 ) made of aluminum oxide is surrounded, which fit snugly into each other. 2. Probentisch nach Anspruch 1, dadurch gekennzeichnet, daß der Heizdraht (7) bifilar gewickelt und parallel zum Elektronenstrahl angeordnet ist.2. Sample table according to claim 1, characterized in that the heating wire ( 7 ) is wound bifilarly and is arranged parallel to the electron beam.
DE1997129526 1997-07-10 1997-07-10 Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures Expired - Fee Related DE19729526C2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
DE1997129526 DE19729526C2 (en) 1997-07-10 1997-07-10 Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
DE1997129526 DE19729526C2 (en) 1997-07-10 1997-07-10 Heated sample table for in-situ imaging in scanning electron microscopes at high temperatures

Publications (2)

Publication Number Publication Date
DE19729526A1 DE19729526A1 (en) 1999-01-14
DE19729526C2 true DE19729526C2 (en) 1999-07-22

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103594310B (en) * 2013-11-22 2015-09-16 北京中科科仪股份有限公司 High temperature secondary electron detector collection assembly and high temperature ESEM

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1131820B (en) * 1961-02-06 1962-06-20 Siemens Ag Heatable object carrier for electron beam devices, especially electron microscopes, and methods for determining the object temperature
DE2753700A1 (en) * 1977-02-11 1978-08-17 Akad Wissenschaften Ddr Thermal deformation tensile test machine - has specimen directly heated at constant temp. and velocity and placed under tension
DE3126575C2 (en) * 1979-06-28 1984-07-26 Nihon Denshi K.K., Tokyo Device for detecting the secondary electrons in a scanning electron microscope
DE3500903A1 (en) * 1985-01-12 1986-07-17 Fa. Carl Zeiss, 7920 Heidenheim DETECTOR FOR REVERSE SCREW ELECTRONES
DE4213381A1 (en) * 1991-05-06 1992-11-12 Bicron Corp BETA SCINTILLATION PROBE
WO1997007526A1 (en) * 1995-08-11 1997-02-27 Philips Electronics North America Corporation High temperature specimen stage and detector for an environmental scanning electron microscope

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1131820B (en) * 1961-02-06 1962-06-20 Siemens Ag Heatable object carrier for electron beam devices, especially electron microscopes, and methods for determining the object temperature
DE2753700A1 (en) * 1977-02-11 1978-08-17 Akad Wissenschaften Ddr Thermal deformation tensile test machine - has specimen directly heated at constant temp. and velocity and placed under tension
DE3126575C2 (en) * 1979-06-28 1984-07-26 Nihon Denshi K.K., Tokyo Device for detecting the secondary electrons in a scanning electron microscope
DE3500903A1 (en) * 1985-01-12 1986-07-17 Fa. Carl Zeiss, 7920 Heidenheim DETECTOR FOR REVERSE SCREW ELECTRONES
DE4213381A1 (en) * 1991-05-06 1992-11-12 Bicron Corp BETA SCINTILLATION PROBE
WO1997007526A1 (en) * 1995-08-11 1997-02-27 Philips Electronics North America Corporation High temperature specimen stage and detector for an environmental scanning electron microscope

Also Published As

Publication number Publication date
DE19729526A1 (en) 1999-01-14

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OP8 Request for examination as to paragraph 44 patent law
8122 Nonbinding interest in granting licenses declared
D2 Grant after examination
8380 Miscellaneous part iii

Free format text: DIE BEZEICHNUNG IST ZU AENDERN IN: BEHEIZBARER PROBENTISCH ZUR IN-SITU ABBILDUNG IN RASTERELEKTRONENMIKROSKOPEN BEI HOHEN TEMPERATUREN

8364 No opposition during term of opposition
8339 Ceased/non-payment of the annual fee