Difference between revisions of "Hot Gas Blower (Cyberstar)"
| Line 45: | Line 45: | ||
Nominal (Set) Temperature Observed Temperature Set - Obs | Nominal (Set) Temperature Observed Temperature Set - Obs | ||
deg C deg K deg C deg K deg | deg C deg K deg C deg K deg | ||
25 298 25 295 0 | 25 298 25 295 0 | ||
100 373 93 366 -7 | 100 373 93 366 -7 | ||
200 473 188 461 -12 | 200 473 188 461 -12 | ||
300 573 283 556 -17 | 300 573 283 556 -17 | ||
400 673 378 651 -22 | 400 673 378 651 -22 | ||
500 773 472 745 -28 | 500 773 472 745 -28 | ||
600 873 567 840 -33 | 600 873 567 840 -33 | ||
700 973 662 935 -38 | 700 973 662 935 -38 | ||
800 1073 757 1030 -43 | 800 1073 757 1030 -43 | ||
900 1173 852 1125 -48 | 900 1173 852 1125 -48 | ||
950 1223 899 1172 -51 | 950 1223 899 1172 -51 | ||
Revision as of 22:47, 24 September 2012
About
11-BM has a dedicated Cyberstar Hot Gas Blower. This can be used to heat small diameter capillary samples from ambient temperature to ~ 950 °C
About
Temperature Range and Ramp Rate.
- ambient temperature to ~ 950 °C
- Max ramp rate on heating & cooling is 5 deg C/min (300 C/hour)
Users should plan experiments to incorporate these heating and cooling ramp times.
11-BM Hot Gas Blower Image
Temperature Profile & Alignment
Temperature Calibration
Al2O3 Thermal Expansion
In-situ calibration of the hot gas blower was performed using the known thermal expansion of Al2O3 alumina a & c unit cell parameters as a function of temperature.
Full powder diffraction patterns were collected for select "nominal" set temperatures between 100 - 950 C at 11-BM using a X.X mm diameter fused quartz capillary load with ??? Al2O3 powder.
Refinements were performed against data from each nominal temperature to determine a & c unit cell parameters.
Based on the initial room temperature 25 C lattice values and published thermal expansion equations (below, see Reference 1), "real" observed sample temperatures were then calculated independently for each set of 'a & c unit cell terms.
The thermal expansion equation used for the a axis of Al203 (range 293-1900 K) is:
delta(a)/a (%) = -0.176 + (5.431E-4 * T) + (2.150-7 * T^2) - (2.810E-11 * T^3) (T/K) assuming a room-temperature lattice parameter of a = 4.7592 A
The thermal expansion equation used for the c axis of Al203 (range 293-1900 K) is:
delta(c)/c (%) = -0.192 + (5.927E-4 * T) + (2.142E-7 * T^2) - (2.207E-11 * T^3) (T/K) assuming a room-temperature lattice parameter of c = 12.9934 A
Finally, plotting observed vs nominal set temperatures for the Al2O3 data gives a correction curve and equation for other hot air blower measurements at 11-BM under similar experimental conditions.
These results (from July 2012) are shown below. These calibration data are kindly shared by Jae-Hyuk Her, GE Global Research.
Nominal (Set) Temperature Observed Temperature Set - Obs deg C deg K deg C deg K deg 25 298 25 295 0 100 373 93 366 -7 200 473 188 461 -12 300 573 283 556 -17 400 673 378 651 -22 500 773 472 745 -28 600 873 567 840 -33 700 973 662 935 -38 800 1073 757 1030 -43 900 1173 852 1125 -48 950 1223 899 1172 -51
Reference 1 = J. Appl. Cryst. (1993). 26, 77-81
Phase Transitions
SiO2
PbTiO3
