CS276342B6 - Method of elemental microanalysis of layered structures - Google Patents

Method of elemental microanalysis of layered structures Download PDF

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CS276342B6
CS276342B6 CS855722A CS572285A CS276342B6 CS 276342 B6 CS276342 B6 CS 276342B6 CS 855722 A CS855722 A CS 855722A CS 572285 A CS572285 A CS 572285A CS 276342 B6 CS276342 B6 CS 276342B6
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layered structures
depth
microanalysis
distribution
elemental microanalysis
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CS855722A
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Czech (cs)
Slovak (sk)
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CS572285A3 (en
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Kornel Rndr Csc Csach
Jozef Csc Miskuf
Vojtech Prof Ing Drsc Karel
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Ustav Ex Fyziky Sav
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Priority to CS855722A priority Critical patent/CS276342B6/en
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Publication of CS276342B6 publication Critical patent/CS276342B6/en

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Abstract

Využitie zmien podmienok mikroanalýzy charakteristického róntge- nového žiarcnia v rastrovacom elektrono- vom mikroskope pre získanie informácií o prvkovej distribúcii nehomogenních vrstevnatých štruktúr. To Sa zistuje v hlbke 0,5 .um, pri uhle snímania do 30° pri náklone vzorky nad 45° a urých- íovacom napatí do dvojnásobku excitač- nej energie prvku. ípósob mikroanalýzy. je možné použit všade tam, kde je potřebné zistit híbkovú distribúciu prvkov.vrstevnatých štruktúr v inter- - vale híbky 1 nm až 0,5 .um od po ­vrchu.The use of changes in the conditions of microanalysis of characteristic X-ray radiation in a scanning electron microscope to obtain information about the elemental distribution of inhomogeneous layered structures. This is determined at a depth of 0.5 .um, at a scanning angle of up to 30°, with a sample tilt of over 45° and an accelerating voltage of up to twice the excitation energy of the element. The microanalysis method can be used wherever it is necessary to determine the depth distribution of elements of layered structures in the depth interval of 1 nm to 0.5 .um from the surface.

Description

Vynález sa týka spôsobu prvkovej mikroanalýzy vrstevnatých štruktúr.The invention relates to a method of elemental microanalysis of layered structures.

Zo zmeny podmienok mikroanalýzy pomocou charakteristického rontgenového žiarenia na rastrovacom elektrónovom mikroskope sa získajú informácie o prvkovej distribúcii nehomogénnych vrstevnatých štruktúr.From the change of microanalysis conditions by characteristic X-ray radiation on the scanning electron microscope, information about the elemental distribution of inhomogeneous layer structures is obtained.

Pre získanie informácií o hĺbkovej distribúcii prvkov v pevných látkach Sa používajú predovšetkým chemické a fyzikálne postupy spočívajúce v analýze tenkých povrchových oblastí pri postupnom odstraňovaní povrchových vrstiev. Spoločným nedostatkom týchto metód je ich deštruktívny charakter spočívajúci v odstraňovaní analyzovanej oblasti. Použitie kolmých, resp. šikmých rezov vrstevnatého materiálu je viazané na použitie lokálnej mikroanalýzy o veími malom analyzovanom objeme.In particular, chemical and physical procedures involving the analysis of thin surface areas for the gradual removal of surface layers are used to obtain information about the depth distribution of elements in solids. A common drawback of these methods is their destructive nature of removing the analyzed area. The use of perpendicular, respectively. oblique cuts of layered material are bound to the use of local microanalysis of a very small analyzed volume.

Uvedené nevýhody sú odstránené použitím prvkovej mikroanalýzy vrstevnatých štruktúr pre získanie informácií o hĺbkovej distribúcii prvkov v nehomogénnych vrstevnatých Štruktúrach podl-a vynálezu.These disadvantages are eliminated by using elemental microanalysis of layered structures to obtain information about the depth distribution of elements in the non-uniform layered structures of the invention.

Jeho podstatou je spôsob prvkovej mikroanalýzy vrstevnatých štruktúr pri ktorom sa zistuje hĺbková distribúcia prvkov vrstevnatých štruktúr v hĺbke do 0,5 yum pri uhle snímania do 30°, pri náklone vzorky do 45° a urychíovacej energií elektrónového zväzku do dvojnásobku excitačnej energie sledovaného prvku.Its essence is a method of elemental microanalysis of stratified structures in which a depth distribution of elements of layered structures at depths up to 0.5 yum is found at a scanning angle of up to 30 °, at a tilt of the sample up to 45 ° and an accelerating energy of the electron beam up to twice the excitation energy of the observed element.

Využíva sa tak zmena geometrických podmienok a energie primárnych elektrónov pri mikroanalýze. Pri zmene urychíovacieho napätia primárneho elektrónového, lúča, uhla dopadu primárnych elektrónov a uhla snímania emitovaného rontgenového žiarenia sa zákonitým spôsobom mení intenzita snímaného charakteristického rontgenového žiarenia sledovaných prvkov. Z charakteru týchto zmien možno usudzoval: na distribúciu sledovaných prvkov od povrchu pevných látok smerom dovnútra vzorky, predovšetkým v oblasti 1 nm &ž U,5 yum. PríkladThus, a change in the geometrical conditions and energy of the primary electrons is used in microanalysis. When changing the accelerating voltage of the primary electron, the beam, the angle of impact of the primary electrons and the scanning angle of the emitted X-ray radiation, the intensity of the sensed X-ray radiation of the monitored elements is changed in a regular way. From the nature of these changes it may be thought: to distribute the elements to be monitored from the surface of the solids to the inside of the sample, especially in the 1 nm & Example

Pomocou rastrovacieho elektrónového mikroskopu Tesla 0Ξ 300 a EDX analyzátora EDAX 3100/60 bola meraná závislost intenzity P,,„ žiarenia emitovaného z povrchu vzorky ocele ' , Iv , v , s ionovo implantovaným fosforom . dávky 10 _ ionov/cnT od urýchlovacieho napatia elektrónového zväzku v intervale 7 až 20 kV, pri prúde zväzku 6,5 . 10 Λ. Pri kon-štantnom urýchíovacom napätí 12 kV bola meraná uhlová závislost intenzity žiarenia.The scanning electron microscope Tesla 0-300 and the EDX analyzer EDAX 3100/60 measured the dependence of the intensity of the radiation emitted from the surface of the steel sample, IV, v, with the ion-implanted phosphorus. 10-ion / cnT dose from electron beam acceleration voltage in the range of 7 to 20 kV, at beam current 6.5. 10 Λ. At a constant acceleration voltage of 12 kV, the angular dependence of the radiation intensity was measured.

Zmena uhla snímania emitovaného žiarenia bola dosiahnutá rotováním vzorky okolo zvislej osi. Uhol medzi rovinou vzorky a osou rotácie bol zhodný s elevačným uhlom detektora (v danom prípade 35°). Týmto spôsobom bol určený koncentračný gradient fosforu do hĺbky 0,3 /um od povrchu vzorky.Changing the scanning angle of emitted radiation was achieved by rotating the sample around the vertical axis. The angle between the plane of the sample and the axis of rotation was identical to the elevation angle of the detector (in this case 35 °). A phosphorus concentration gradient of 0.3 µm from the sample surface was determined in this way.

Uvedený spôsob analýzy podía vynálezu možno využit všade tom, kde je potrebné nedeštruktívnym spôsobom zistil hĺbkovú distribúciu prvkov, ktoré sú detekovateíné využívanou metódou. Využíva sa nájdená možnost plynulej zmeny uhla snímania emitovaného rontgenového žiarenia aj keď detektor žiarenia je v elektrónovom mikroskope fixne zabudovaný.This method of analysis of the invention can be utilized wherever the depth distribution of the elements detectable by the method used has to be determined in a non-destructive manner. The possibility of continuously changing the scanning angle of the emitted X-ray radiation is used, although the radiation detector is fixed in the electron microscope.

Claims (1)

PATENTOVÉPATENT Spósob prvkovej mikroanalýzy vrstevnatých štřuktúr pre nedešťruktívne zistenie' prvkovej distribúcie nehomogénnych vrstevnatých štřuktúr změnou geometrických podmienok a energie, vyznačujúci sa tým, že híbková distribúcia prvkov sa zistuje v híbke doMethod of elemental microanalysis of stratified structures for non-destructive detection of elemental distribution of non-homogeneous stratified structures by changing geometric conditions and energy, characterized in that the in-depth distribution of elements is detected in depth 0,5 yum pri uhle snímania do 30°, pri náklone vzorky do 45° a urýchíovacom -napatí elektronového zvázku do dvojnásobku excitačnej energie prvku.0.5 yum at a scanning angle of up to 30 °, a sample tilting up to 45 ° and an accelerating-electron beam voltage up to twice the element's excitation energy.
CS855722A 1985-08-06 1985-08-06 Method of elemental microanalysis of layered structures CS276342B6 (en)

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