Journal of Magnetismand MagneticMaterials41 (1984) 247-249 North-Holland,Amsterdam

247

A SENSITIVE VIBRATING SAMPLE MAGNETOMETER

R. BERANEK and C. HEIDEN

Institut fiir A ngewandte Physik der Justus- Liebig-Unioersiti~t Giessen, D 63 Giessen, Fed. Rep. Germany

A sensitive vibrating sample magnetometeris described allowing magnetizationmeasurements on samples with small dimensionsin fieldsup to 2 T and temperaturerangebetween2 and 300 K.
1. Introduction

Many efforts have been reported over the last few years to construct magnetometers with increased sensitivity [1]. This has been achieved by using lock-in techniques as in the vibrating reed magnetometer [2] or by using the high-flux sensitivity of a superconducting quantum interference device (SQUID) [3-9]. In this paper we describe a vibrating sample magnetometer with a SQUID-detector, which was developed for measurements on small specimens over a temperature range between 2 and 300 K. Lock-in technique is used for noise reduction in order to compensate for the loss of sensitivity due to the space needed for thermal insulation which reduces the magnetic coupling between sample and pickup loop of the SQUID.
2. Details of construction

consists of a thin-walled German silver Tube GT i with a diameter of 1.5 mm. A bifilar manganin heater H of 300 fl is wound on this tube. To monitor the temperature a small Ga-As-diode TS is mounted in the specimen chamber. The thermal coupling between sample, heater and temperature sensor is made by helium gas. The temperature of the sample can be raised to room temperature in about 30 s. By the tube GT v the sample Dewar can be connected to the surrounding liquid helium cryostat via a throttle valve (not shown), which allows quick lowering of the temperature down to 4.2 K. By pumping the He-dewar, sample tempera1
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Vibrating Capacitor i

The scheme of the magnetometer system is indicated in fig. 1. The sample holder consists of a thin quartz tube of ca. 0.5 mm diameter, which is fixed to a long (ca. 1 m) thin walled German silver tube. The whole setup is driven by the transducer of a commercial vibrating sample magnetometer (PAR model 155) with a vibration frequency of ca. 80 Hz. A gradiometer configuration is used for the pickup loop to couple the flux to a commercial rf-SQUID (S.H.E. System 330). The output of the SQUID electronics is connected via a filter and phaseshifter to the phase sensitive detector of the lock-in system of the vibrating sample magnetometer. A special circuit provides compensation for variations of the vibration amplitude. Fig. 2 shows details of part of the system immersed in liquid helium. The specimen chamber

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i
J
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I I

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0304-8853/84/$03.00 Elsevier Science Publishers B.V. (North-Holland Physics Publishing Division)

248 ~jGTi

R. Beranek and C. Heiden / .4 sensitive vibrating sample magnetometer

pickup coils, as depicted also in fig. 2, is chosen such as to minimize the sensitivity of the system with regard to variations in the average sample position [10].

3. System performance

1
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Fig. 2. Cross section of system immersed in liquid helium. Pickup coil configuration is shown enlarged at fight.

tures down to 2.0 K can be reached easily. The outer German silver tube G T o has a constriction of 3.4 mm diameter for the two astatic pickup loops. The space between the inner and outer tube, which is sealed by the chambers CC and VC, respectively, is evacuated and filled with superinsulation for thermal insulation between sample and helium bath. Plastic spacers Sp1 are used to maintain the radial alignment of G T i and G T o. Centered by spacers Sp2, the tube G T o is rigidly cast in the bore of a block of epoxy ER filled with an appropriate amount of quartz powder for thermal expansion matching. The epoxy block also acts as support structure for the pair of Helmholtz coils F. Vibrations of the pickup coils relative to the magnetization field are thereby minimized. The Helmholtz coils are constructed with NbTi-wire and allow application of fields up to 2 T at the sample. The pickup coil system is designed for maximum coupling to the SQUID, i.e. the inductance of the astatic pair of coils equals the SQUID input inductance. This results in two coils with 10 windings respectively with an inner diameter of 3.4 mm to give an inductance together with the twisted wires in the tube LT leading to the SQUID of ca. 1.8 rtH. The whole flux transfer circuit is made of 0.1 mm insulated NbTi-wire. The geometry of the

Using a totally superconducting flux transfer circuit, it is not possible to record continuously the whole magnetization curve of a sample during field sweeps. Imperfect compensation of the detection coil system for homogeneous fields and the limited dynamic range ( + 500 flux quanta) leads to overloading of the SQUID system. To overcome this problem a small resistor is inserted in the flux transfer circuit, which then shows the frequency behavior of a high-pass filter. Slow variations of the applied field are no longer coupled to the SQUID. The value of the resistor has to be chosen such that the signal at the vibration frequency of 80 Hz is not markedly decreased and that the Johnson noise of the resistor does not dominate over other noise sources. A small copper wire therefore is used with a resistance of about 1 m[L The magnetometer was calibrated using a superconducting lead sphere of ca. 200 r: m diameter in the Meissner state. The dimensions were determined by a scanning electron microscope, allowing calculation of the magnetic moment of the ideal diamagnet. The ultimate flux sensitivity of the given SQUID is limited by its intrinsic noise of 2 X 10-. 4 @ 0 / / n ~ : This would correspond to a sensitivity of 2 x 10 -13 Am2//~/nzz for the magnetic moment in our system. The output noise of the calibrated magnetometer for a temperature of 4.2 K is shown in fig. 3. The intrinsic noise of the SQUID is obviously not the limiting factor for sensitivity. At present state changes in magnetic moment slightly less than 1 10-12 Am 2 can be detected using a time constant of the lock-in amplifier of 100 s. Aside from the Cu-resistor in the flux transfer circuit, producing an equivalent thermal moment noise of 8 x 10 -13 A m 2 / H ~ , the walls and the heater of the specimen chamber have to be regarded as sources of thermal noise impairing the performance of the system. An applied field of 500 m T does not markedly decrease the sensitivity at

R. Beranek and C. Heiden / A sensitive vibrating sample magnetometer

249

the electromechanical transducer with regard to the cryostat.

4. Further developments
"~'~"~'~'%~"~'~'-'/'"-........... q,L.,oa. I 2x10-'2Am2' z:100s B=0 ~ ........ 1~ I 2x10-" Am 2. 1;: Is B=I0mT

I 2x 10-t' Am 2. Z = Is

B = I00 rnT

I 2xlO-" Am 2, z :

Is

B = 500 m T

I IOmin

I T= /. 21 K

Fig. 3. Recording of system output noise. 4.2 K. At higher temperatures however the noise of the present system increases with rising field. One likely cause for this are helium bubbles generated around tube GTo due to the heat input to the bath, that amounts to ca. 200 mW at 300 K. A winding technique leading to a better compensation of the detection coils is being developed presently, which should improve the situation. Using a time constant of 1 s, several minutes usually are needed to complete one field sweep in order to obtain the magnetization curve of a specimen. Samples can be changed in less than a minute without warming up the cold part of the system. For this, the sample holder is removed through an opening at the head of the apparatus. A small overpressure of helium gas in the specimen chamber prevents air from leaking in. After removing the former sample, the new one is glued to the thin quartz tube at the lower end of the sample holder. After inserting the latter again into the magnetometer the driving mechanism is switched on and the average sample position is adjusted for maximum output signal by means of changing the position of

Although the sensitivity of the system appears to be quite adequate for specimen temperatures less than ca. 50 K, improvements may be desirable at higher temperatures, especially around room temperature. Apart from the above mentioned better compensation of the pickup coils, one obvious way is to remove as far as possible sources of thermal noise from the flux transfer loop. This m a y be achieved by using plastic specimen chamber made of thin walled fiber glass reinforced epoxy tubes. For this purpose, the heater also may be divided into two parts located at some distance from the pickup loop [11].

References
[1] S. Foner, IEEE Trans. Magn. MAG-17 (1981) 3358. [2] W. Roos, K.A. Hempel, C. Voigt, H. Dederichs and R. Schippan, Rev. Sci. lnstrum. 51 (1980) 612. [3] E.J. Cucauskas, D.A. Vincent and B.S. Deaver Jr., Rev. Sci. Instrum. 45 (1974) 1. [4] M. Cerdonio, C. Cosmelli and G.L. Romani, Rev. Sci. Instrum. 47 (1976) 1. [5] J.S. Philo and W.M. Fairbank, Rev. Sci. Instrum. 48 (1977) 1529. [6] S.E. Nave and P.G. Huray, Rev. Sci. Instrum. 51 (1980) 591. [7] M. Pelizzone and A. Treyvaud, Appl. Phys. 24 (1981) 375. [8] C. Heiden and H. Rogalla, J. Magn. Magn. Mat. 19 (1980) 240. [9] SHE Model 905 VTS Superconducting Magnetometer, SHE Corporation. [10] A. Zieba and S. Foner, Rev. Sci. Instrum. 53 (1982) 1344. [11] S. Stieler and C. Heiden, in: Proc. Ninth Intern. Cryogenic Engineering Conf., eds. K. Yasukochi and H. Nagano (Butterworth, Guildford, 1982) p. 551.