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A Practical Hot Stage for High Temperature

Micro-Analysis

Ralph G. Tissot Jr. and Mark Rodriguez 1822 Microstructural Characterization Department

Sandia National Laboratories Albuquerque, New Mexico USA 87185

Abstract An understanding of high temperature kinetics and phase transformation in thin film structures is important in microelectronic component production. In order to study these devices at elevated temperatures a microscope hot stage was modified for high temperature microdiffraction analysis. With minor modifications, surface temperatures of 1OOOCand greater could be reached rapidly and with reliable steady state operation. This paper will discuss the heater modifications, temperature control and cooling requirements as well as examples of high temperature micro-analysis. Introduction A method for obtaining high temperature information from micro-areas on small electronic thin-film devices was needed. Therefore a hot stage was required that 1) could be mounted vertically on an XYZ stage, 2) was physically small and robust with easy access to the heated surface, 3) could reach surface temperatures in excess of 850C rapidly while maintaining temperature stability and 4) could be used in close proximity with x-ray capillary optics . A Leitz Model 1350 microscope heating stage with minor design modifications was found to be ideal [ 11. This hot stage with its rapid temperature rate exhibited excellent high temperature (I: 1C @ SSOC) stability and clearly demonstrated its versatility for use with most any system requiring high temperature micro-analysis. Hot Stage Modifications The microscope heating stage is a water-cooled Leitz Model 1350 with a maximum heating temperature of 13 50C at 18A (Fig. 1). The stage dimensions are 85mm in diameter and 35mm in height. Two clamping screws provide a means of mounting the heater to a diffractometer stage. Also centering screws provide both XY orientation and for aligning the sample surface normal to the incident x-ray beam. Inlet and outlet ports provide both cooling water and the use of various protective gases, i.e. argon. A stainless steel sample holder and leaf spring provides good sample contact to the heated surface.

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Minor modifications were made to enhance the hot stage performance for micro-analysis using a XYZ diffractometer stage. A 38mm long platinum strip lmm thick and 1Omm wide was fashioned to placed over the heater core (Fig.2). A small hole slightly larger than the diameter of a thermocouple bead was drilled from the bottom of the platinum strip to a point near the surface below where the sample would be placed. A Type K (0.020 in. diameter) thermocouple was used. Once the bead was centered in the hole, a small center punch was used to peen close the hole around the thermocouple bead. This method of thermocouple placement provides an easier means of thermocouple replacement and allows better temperature monitoring of the heater core. The thermocouple leads are than feed through the center of the heater core and the platinum strip positioned before encapsulating with insulation. The insulation used was a ceramic refractory wool suitable for high temperature. The insulation is packed below the heater core and around the platinum strip Caution should be used to insure that the platinum heating coils do not touch the platinum strip. Temperature Control

Heater temperatures measured by the peened thermocouple were controlled using a Honeywell Dialatrol 2OOOOFon/off controller coupled with a variable autotransformer for varying current output to the heater. Current and voltage analog gages were used to obtain current and voltage readings respectively. Typically the current is set to a value for a given heater temperature. In this way the heater is operated at constant power with no on/off switching, thus providing uniform heating throughout the analysis. Sample temperatures were monitored by positioning a 0.010 in. diameter Type K thermocouple on the sample surface with the temperature recorded on a digital readout. Caution should be used with Platinum- based thermocouples in contact with silicon or silicon dioxide because of thermocouple instability and failure at elevated temperatures [2]. Surface temperatures can be calibrated using melting point standards versus applied current settings if desired.

Fig. 1 Microscope heating stage

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Thin film samplt+

@mface thermocouple

Fig.2 Schematic showing Platinum strip, heater core and thermocouple position.

Cooling Requirements The cooling requirements were found to be very minimal. For analysis requiring short times no cooling is required; for longer times (> 1 hour) cooling is recommended especially at very high temperatures. For our purposes a Cole Parmer peristaltic pump was used to circulate cooling water from a 1 liter reservoir. This system was more than adequate for longer analysis times and higher temperatures. Heater Performance The heater current was set for 10 amps and allowed to reach temperature equilibrium. Surface temperature was monitored on a 1Omm square sample of silicon (100) single crystal. Figure 3 shows a time/temperature plot of the surface and heater core temperatures. The maximum heater temperature of 850C at 10 amps was reached in approximately 4 minutes. The stability after 6 minutes was f 1C resulting in constant temperature difference between sample and heater of 150C. A consistent temperature lag was also observed. With higher amperage settings, it was possible to achieve sample surface temperatures of 900C. Temperature differences of course will vary depending on heater temperature used.

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Hot Stage Performance

1OOOl I I I I I ( ) 1

800 -

600 -

2 d k 400 B F 200 t Iot n 2:oo 4:oo 6:00 8:00 TIME (mid 1o:oo

Fig.3 Hot Stage Performance

Testing The instrumentation used to obtain diffraction patterns was a Rigaku 12kW rotating Cu anode, a 10 micron total reflection tapered glass capillary coupled with a Siemens goniometer. The goniometer was equipped with XYZ translation stage and a Siemens HiStar area detector. Both samples were analyzed at 50kV lOOmA at a sample to detector distance of 8.5 cm with each pattern collected for 300 sec. A nickel filter was employed for Cu kp removal. In order to test the hot stage a polycrystalline silver [3] metal film deposited on an alumina polycrystalline substrate was heated to a surface temperature of 850C. Area scans were taken at 100C from 300C to 800C. This sample clearly showed an increased spottiness in the pattern beginning at 700C and becoming almost entirely spots at 850C; indicative of grain growth due to annealing (Fig.4).

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Fig.4 Silver metal film showing grain growth from annealing. Summary Clearly, using a microscopic hot stage with minor modifications brings a versatility to high temperature microanalysis. Its simplicity and robustness allows ease of mounting and removal of the hot stage to most any diffractometer or synchrotron sample stage in either vertical or horizontal positions. The small heating area allows the placement of total reflecting collimators nearer to the sample without damage to the glass capillary. Small samples can be examined with a more uniform temperature distribution and faster temperature response allowing the study of materials exhibiting rapid high temperature kinetics. Acknowledgments This work was performed at Sandia National Laboratories operated by Sandia Corporation, a Lockheed Martin Company, for the United States Department of Energy under Contract DE-ACO4-94AL85000. References 1. Instructions: Microscope Heating Stage Leitz 1350, Leica Inc. Deer-field, IL (1990) 2. Pollock, D.D., Thermocouples: Theory and Properties, CRC Press, Boca Raton pg. 220 (1991) 3. Ag, PDF#O4-0783, ICDD, Newton Square, PA.; Swanson, Tatge, Nat.Bur.Std. (U.S.) Cir. 53 1,123(1953)