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INSTRUMENTATION, ELECTRON OPTICS AND X-RAY SPECTROSCOPY
T. Mulvey
To cite this version:
T. Mulvey. INSTRUMENTATION, ELECTRON OPTICS AND X-RAY SPECTROSCOPY. Journal
de Physique Colloques, 1984, 45 (C2), pp.C2-149-C2-154. �10.1051/jphyscol:1984233�. �jpa-00223946�
JOURNAL DE PHYSIQUE
Colloque C2, supplément au n°2, Tome 45, février 1984 page C2-149
INSTRUMENTATION, ELECTRON OPTICS AND X-RAY SPECTROSCOPY
T. Mulvey
Department of Physios, The University of Aston in Birmingham, B4 7ET, U.K.
Résumé - Les développements récents dans le champ d'instrumentation du micro- analyseur à rayons X sont revus, ainsi que les canons électroniques, les systèmes des lentilles et les détecteurs des électrons rétrodiffusés (Z contraste). Les amé- liorations souhaitables pour l'analyse des échantillons minces à l'aide de la spec- trométrie à dispersion en énergie sont aussi discutées.
Abstract - Recent instrumental developments in the field of electron probe instrumentation are reviewed. These include electron guns, lens systems and back-scattered electron (Z contrast) detectors. Desirable changes in instrumental design are discussed for the analysis of thin specimens by the use of energy dispersive spectrometers.
1 - INTRODUCTION
The present symposium is concerned with recent developments in all aspects of electron instrumentation of electron probe X-ray microanalysis. It is perhaps interesting to note that the initial stimulus to develop the electron probe micro- analyser was the early discussions between Castaing and Guinier in the period 1947-1948 as to whether it was possible to analyse by X-ray spectrometry the fine detail visible at that time in thin metallic specimens in the electron microscope.
It was of course necessary to begin with the more modest resolution set by the light microscope. After a period of some thirty years of development, microanalysis of this type has now reached a high stage of technological development especially with the recent introduction of microprocessor and mini-computer control. Nevertheless, further development is still possible, especially in the choice and control of X-ray spectrometers. On the other hand, recent progress in atomic resolution transmission electron microscopy (TEH) and the development of high resolution analytical scanning transmission microscopes (STEM) has made it desirable to review the instrumental techniques used in X-ray analysis of thin specimens at high spatial resolution
( = 2 nm) .
These include, among others, the elimination from the detector of all X-rays not emanating from the specimen area under investigation and the handling of the greatly increased amount of analytical data produced by the modern analytical STEM. In addition, it is desirable to be able to correlate the analytical information from the characteristic X-ray emission with that from Auger and energy loss spectroscopy and perhaps from convergent beam diffraction, which combines the high spatial reso- lution of electron probe analysis with crystallographic information not available with any other X-ray diffraction technique,
The increasing computer automation that is available today also calls for an
approach to instrumentation that eliminates, as far as possible, intervention by the operator in setting up and aligning the instrument and the recognition of
instrumental artefacts arising during the analysis.
Improved methods of detection of light elements in low concentrations and the increased ability to examine thin surface layers have recently emphasized the need to improve, by a few orders of magnitude, the traditional poor vacuum ( - 10 mbar)
Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1984233
JOURNAL DE PHYSIQUE
of many X-ray microanalysers. Here t h e i n t r o d u c t i o n of turbo-molecular pumps, t h e a v a i l a b i l i t y of improved d i f f u s i o n pump o i l s , and t h e i n s e r t i o n of e f f i c i e n t t r a p s i n backing pump l i n e s has done much t o reduce t h e hydrocarbon c o n t e n t of t h e r e s i d u a l g a s e s i n t h e system. Such improved vacuum systems a l s o make it p o s s i b l e t o r e p l a c e t h e t r a d i t i o n a l t u n g s t e n f i l a m e n t by, f o r example, a lanthanum hexaboride cathode with a s u b s t a n t i a l improvement b o t h i n e l e c t r o n o p t i c a l b r i g h t n e s s and f i l a m e n t l i f e . STEM i n s t r u m e n t s need f i e l d emission cathodes and hence w i l l be designed f o r a vacuum p r e s s u r e i n t h e r e g i o n of lo-'' mbar. Such guns were
o r i g i n a l l y designed f o r t h e p r o d u c t i o n of nanometre probes and so a r e n o t e f f i c i e n t f o r producing an adequate c u r r e n t i n t h e l a r g e r probes needed f o r a n a l y t i c a l work.
F u r t h e r development i s however p o s s i b l e .
A
v a l u a b l e a n c i l l a r y development i s t h e high energy b a c k s c a t t e r e d e l e c t r o n o r
' 2c o n t r a s t ' d e t e c t o r whose o u t p u t i s p r o p o r t i o n a l t o t h e average atomic number of of t h e specimen. When made i n t h e form o f f o u r a d j a c e n t q u a d r a n t s , s o a s t o e l i m i n a t e t o p o g r a p h i c a l c o n t r a s t , a r a p i d p r e l i m i n a r y a n a l y s i s can be made of t h e average atomic number of t h e main c o n s t i t u e n t s of t h e specimen.
2 - ELECTRON GUNS
The c u r r e n t d e n s i t y
0of emission from t h e h e a t e d cathode wire i s given by t h e Richardson e q u a t i o n
(1)
0 =A
T~exp (-e @ /k T) ,
where
Ai s a c o n s t a n t f o r a given e m i t t i n g m a t e r i a l , T i s t h e a b s o l u t e temperature, k i s Boltzmann's c o n s t a n t and @ i s t h e 'work f u n c t i o n ' o f t h e m a t e r i a l expressed i n
' e l e c t r o n v o l t s ' . The maximum b r i g h t n e s s ( R i c h t s t r a h l w e r t ) B of t h e r e s u l t i n g e l e c t r o n beam a f t e r a c c e l e r a t i o n through a p o t e n t i a l d i f f e r e n c e V i s given approxi- mately by
The work f u n c t i o n of t u n g s t e n i s i n c o n v e n i e n t l y l a r g e , approximately 4.5 eV, b u t t h i s can be reduced by t h e Schottky e f f e c t , by which a s t r o n g e l e c t r i c f i e l d of s t r e n g t h E a t t h e cathode s u r f a c e enhances t h e emission c u r r e n t d e n s i t y
0by a f a c t o r exp(0.44 E / T ) . f Here
Ei s measured i n v o l t s / m e t r e . This f i e l d can be most c o n v e n i e n t l y produced by forming a f i n e p o i n t on t h e e m i t t i n g s u r f a c e . Thus Van d e r Mast e t a l . /1/ succeeded i n producing a l a s e r - h e a t e d Schottky thermionic source t h a t i s comparable i n performance w i t h a f i e l d emission e l e c t r o n gun, b u t does n o t need a p a r t i c u l a r l y good vacuum. I n a d d i t i o n it i s c a p a b l e of d e l i v e r i n g t h e l a r g e r probe c u r r e n t s t h a t a r e needed f o r a n a l y t i c a l work. I n t h i s source ( F i g . 1) a t h i n t u n g s t e n wire of some 1 0 w i n diameter i s h e a t e d l o c a l l y a t i t s t i p t o a
temperature n e a r i t s melting p o i n t . An e l e c t r o d e a t a p o s i t i v e p o t e n t i a l p o s i t i o n e d near t h e source c r e a t e s t h e e l e c t r i c f i e l d needed f o r enhanced Schottky emission.
Under t h e i n f l u e n c e of t h i s f i e l d and s u r f a c e t e n s i o n a s t a b l e e m i t t e r of f i x e d small r a d i u s of c u r v a t u r e i s produced. A s t h e cathode wire i s evaporated t h e wire i s f e d i n t o t h e l a s e r focus t o p r o v i d e t h e necessary replacement. The measured b r i g h t n e s s of t h i s s o u r c e i s i n t h e r e g i o n of 8
X10' A/cm2/sterad. a t 25 kV, comparable with t h a t of a f i e l d emission gun. This e l e c t r o n gun i s n o t y e t
a v a i l a b l e commercially b u t i t s performance i n d i c a t e s t h a t expremely high b r i g h t n e s s can be produced i n e l e c t r o n guns w i t h t u n g s t e n f i l a m e n t s /2,3/ i f t e c h n o l o g i c a l problems can be s o l v e d .
I tshould perhaps b e p o i n t e d o u t t h a t t h e gun b r i g h t n e s s a s measured under o p e r a t i n g c o n d i t i o n s is n o t n e c e s s a r i l y t h e maximum b r i g h t n e s s a s d e f i n e d i n Equation ( 2 ) b u t r a t h e r a 'mean b r i g h t n e s s ' /4/ a s l i m i t e d , f o r example, by t h e t o t a l cathode c u r r e n t t h a t may be drawn from t h e power supply o r a p a r t i c u l a r arrangement of l e n s a p e r t u r e s . I n g e n e r a l t h e b r i g h t n e s s of an e l e c t r o n gun
improves a s t h e work f u n c t i o n and r a d i u s of t h e cathode i s reduced /5/, a s t h e
t o t a l c u r r e n t i s i n c r e a s e d and a s t h e vacuum i s made b e t t e r . These requirements a r e
n o t e a s i l y s a t i s f i e d simultaneously and economically i n commercial equipment.
A tp r e s e n t t h e t r e n d is towards t h e u s e of lanthanum hexaboride a s a s u b s t i t u t e f o r t h e
t u n g s t e n cathode.
Acomprehensive review of t h e u n d e r l y i n g t h e o r y and measurement
WEHNELT
lUNGSTEN W I R E F E E D MECHANISM
ANODE /I
HIGH B R I G H T N E S S ELECTRON BEAM
I
FOCUSED L A S E R BEAM
MODULATOR
S H I E L D
LABs ROD
HEAT S I N K
Fig.1 Schottky-assisted thermionic emission cathode with laser
Fig.2 Schematic diagram of LaB6 rod cathode
heating
G R A P H I T E BLOCK
Fig.3 Schematic diagram of mechanical clamping of LaB6 crystal between graphite blocks
CARBON ARCH
LAB6 CRYSTAL\
@