Revista Brasileira de Física, Vol.

6, AIQ 1, 1976

A Liquid Nitrogen Cryostat for Optical and X-Band Electron

Spin Resonance Measurements

J.P. v o n der WEID

Departamento de Física, Pon tifícia Universidade Católica ', Rio de Janeiro RJ

Recebido em 3 d e Outubro d e 1975

A sirnple and v e r s a t i l e l i q u i d n i t r o g e n c r y o s t a t i s d e s c r i b e d . The cha-

racteristics of t h e systern are presented, and t h e o p e r a t i o n o f t h e
systern for o p t i c a l and e l e c t r o n s p i n resonance (EsR) measurements,with
t h e sample i n vacuurn, i s described.

Apresenta- se c r i o s t a t o , s i m p l e s e v e r s a t i 1, para n i t r o g ê n i o 1í q u i d o .
Di scutem-se suas c a r a c t e r í s t i c a s e descreve- se a operação do sistema
para medidas Ó p t i c a s e de ressonância e l e t r ô n i c a de s p i n em amostras
em vácuo.

I n s o l i d state investigations, especially i n color centers research,it

i s o f t e n u s e f u l t o make o p t i c a l and ESR rneasurernents o f an irradiated
sample,, a t low temperature, w i t h o u t warming i t up. We r e p o r t h e r e on
a l i q u i d n i t r o g e n temperature c r y o s t a t designed f o r such measurernents
i n s o l i d samples. Other advantages o f t h i s system a r e i t s g r e a t ver-
s a t i l i t y and s i m p l e e x e c u t i o n .

The dewar i s conceived t o f i t e i t h e r a V a r i a n V 4533 X-band rotating

c a v i t y o r a V a r i a n V 4531 m u l t i purpose c a v i t y . It also f i t s almst
a l l o p t i c a l absorption spectrophotometers.

*
P o s t a l address: Rua Marquês de S.Vicente, 209/263, 20000-Rio de Ja-
n e i ro,RJ.
A d e t a i l e d drawing o f the dewar i s shown i n Fig.1. The v e r t i c a l dimen-
s i o n o f the dewar i s l i m i t e d by the d i s t a n c e between the wave guide
f l a n g e and the top o f the r o t a t i n g c a v i t y . I t s diameter i s such that
i t allows an easy h a n d l i n g i n a 3" gap magnet. I n o r d e r t o f i t the ro-
t a t i n g c a v i t y , and have the maximum a v a i l a b l e volume, the c o l d finger
i s placed o f f center.

The inner and o u t e r vessels a r e made o f copper, and the t o p cover and
i n s u l a t i n g tube a r e made o f s t a i n l e s s s t e e l . The i n s u l a t i n g tube has
t o be t h i n enough i n o r d e r t o minimize thermal conduction through i t ,
b u t n o t so t h i n as t o loose mechanical r i g i d i t y . The thickness used
was between .15 mm and .211 mm. The vacuum p o r t may be of brass o r
o t h e r nonmagnetic m a t e r i a l .

I n o r d e r t o minimize r a d i a t i o n losses, the i n n e r w a l l s must be clean

and p o l i s h e d . Also, t o a v o i d o x i d a t i o n o f the w a l l s , t h e dewar must
be s t o r e d always i n vacuum o r , s t i l l b e t t e r , s i l v e r o r g o l d p l a t i n g o f
t h e inner w a l l s can be made.

The volume o f the LN2 vessel i s 80 cm3, and the precool i n g volume is
about 150 cm3. When the dewar i s pumped t o a vacuum o f the order o f
I O - ~t o r r , the 1 i q u i d n i trogen consumption i s o f 10 cm3 p e r hour. When
the vacuum v a l v e i s closed, the I;N, consurnption increases, as the i n -
n e r vacuum degenerates w i t h time. The t o t a l evaporation o f the l i q u i d
nitrogen, i n t h i s condition, takes about 2 1/2 hours. By usírig about
2 g r o f z e o l i t e absorber i n the inner vessel, and baking the system ,
t h i s time can be extended up t o 4 hours o r more. This d u r a t i o n time
ís u s u a l l y enough f o r o p t i c a l and ESR rneasurements, so t h a t the vacuum
pump may be disconnected d u r i n g the measurements. This b r i n g s a g r e a t
s i m p l i f i c a t i o n i n the sample o r i e n t a t i o n procedure, and an improvement
o f the s i g n a l t o n o i s e r a t i o i n the ESR measurements, as the vacuum
pump always introduces sample v i b r a t i o n i n the c a v i t y .

The dewar can be f i t t e d t o the d i f f e r e n t t a i l s w i t h the sample in

vacuum by means o f t h e " t a i l exchange chamber" shown i n Fig.2. The de-
war under vacuum i s introduced through the top o f the chamber, and t h e
s e a l i n g o - r i n g s a r e then f i t t e d t o the t a i l . When the chamber pres-
 COLD FINGER

Fig.1 - Detailed drawing of the dewar. A 1 1 dimensions are in m.

 L
OPTICAL T A I L

ESR T A I L

\\
1
EXTENSION
ROD
sure i s low enough, the t a i l i s pulled downwards. The top cover o f
t h e chamber i s r o t a t e d t o a new p o s i t i o n , where o t h e r t a i l may be pu-
shed upwards, and f i t t e d t o the dewar. When the o p e r a t i o n i s over,the
vacuum i n t h e chamber i s broken, and the dewar may be brought to the
measurement system. ~ 1 - 1the exchange o p e r a t i o n can be c o n t r o l l e d by
means o f the glass windows i n the chamber w a l l .

As the o p t i c a l t a i l i s n o t c y l i n d r i c a l l y symmetrical, an extension rod

must be used i n o r d e r t o m a i n t a i n the vacuum d u r i n g the vertical mo-
tion. This i s t h e reason f o r the d i f f e r e n t design o f one o f the t a i l
ports. When the exchange o p e r a t i o n i s completed, the e x t e n s i o n rod
may be taken away.

Severa 1 k i n d s o f t a i l s may be conceived f o r u s i n g w i t h t h i s equipment.

The o p t i c a l one i s made w i t h a suprasyl q u a r t z c e l l glued with epoxi
t o an aluminum p i e c e which i s f i t t e d t o the dewar. A thin a 1uminum
t a i l o r one o f glass may be used f o r e l e c t r o n i r r a d i a t i o n exper i ences .
For X - r a d i a t i o n experiments, a Mylar window can be adapted t o a tail
o r t o the chamber i t s e l f , .instead o f one o f the glass windows.

I would l i k e t o thank D r . S. Costa R i b e i r o , M r . L.C. Scavarda do Carro

and M r . A. P r i e t o Picon f o r q u i t e u s e f u l suggestions.