Impedance analyzers

HTF-1100.

High Temperature Furnace

A laboratory furnace used specifically for the electrical characterization of materials and also for heat treatment between ambient temperature and 1100 °C.

A reliable solution for high-temperature material testing

The HTF-1100 is a horizontal laboratory tube furnace dedicated to the electrical characterization of materials and for heat treatment in the range between ambient temperature and 1100 °C.

The HTF-1100 is controlled by MT-Lab software when it is used with  a MTZ-35 impedance analyzer. It can also be controlled manually through the programmable Watlow controller accessible on the front panel of the furnace. This controller facilitates the set-up and consequent monitoring of the furnace temperature during tests.

The furnace accommodates many tubular High Temperature Sample Holders (HTSH-1100). A k-type thermocouple placed in the bottom of the furnace ensures the accurate control and measurement of the furnace temperature.

The HTSH-1100 can operate under controlled environment conditions with inert or active gas (Ar, N2, O2, etc) and with variable pressures up to 2 bar relative. A quartz tube is supplied with the HTSH-1100 for performing measurements under controlled atmospheres. The HTSH-1100 base is fitted with a gas inlet/outlet for gas flow. A safety valve rated at 30 PSI limits the internal gas pressure to a maximum value of 2 bar relative.

 

MT-Lab®

An intuitive and comprehensive software
MT-Lab® is an intuitive and a user-friendly software dedicated to the control of Bio-Logic’s impedance analyzer, the acquisition of the impedance data and the temperature. It also allows the control of many temperature control units:
• High temperature furnace (HTF-1100)
• Intermediate Temperature System (ITS)
• Temperature control systems using Eurotherm 22xx and 35xx series controllers

Open-circuit & short circuit compensation.
MT-Lab® software is provided with a compensation protocol for the compensation of residual impedance due to cell cables and/or sample holders

Specifications

Insulation material: Alumina Fiber

Heating System: Super Kanthal 1350°C wire built in a cement cylinder

Temperature Range: Ambient up to 1100°C

Temperature Controller: PM6 Watlow PID controller

Temperature Sensors: K-Type Thermocouple

Temperature Control Accuracy: Better than +/-1°C

Temperature scan: adjustable (from 0.1 °C/min to 20 °C/min)

Safety Features: Emergency stop button; Buzzer sound alarm; Temperature safety limit

Which communication port should I select to connect HTF-1100 to MT-Lab® software?

First the HTF-1100 has to be connected to MTZ-35 using the provided DB9-DB9 cable. Then, on MT-Lab® software, open “Configuration” window and select the appropriate communication port and click on connect button. The appropriate communication port can be obtained by going to “Control Panel”>”Device Manager”> “Ports (COM & LPT). You can see two virtual communication ports “USB serial port (COM N)” and “USB l serial port (COM N+1)”. Select the one with the low order (COM N) to connect the furnace to MT-Lab software.

I have a big temperature gradient between the furnace temperature and the sample temperature measured by the HTF-1100 and HTSH-1100 thermocouples respectively. What should I do?

HTF-1100 is equipped with a thermocouple for the control of the measurement of the temperature inside the furnace (TTCU)). The HTSH-1100 is equipped with the same thermocouple for the sample’s temperature measurement and monitoring (TSample). If the temperature difference is high and this gradient increases with temperature, check the furnace thermocouple in the bottom of the Inconel shield of the furnace. The end of the furnace thermocouple has to be located inside the Inconel shield of the furnace. If you don’t see it dismantle the Inconel shield, shift slightly the end of the furnace’s thermocouple in a way to be inside the Inconel shield and screw the shield.

I set a setpoint temperature of 700 °C on MT-Lab® software however the furnace heats up to 730 °C why?

The HTF-1100 furnace was designed to accommodate the HTSH-1100 sample holder. Two temperatures are measured: the first one obtained by the furnace thermocouple (TTCU) and the second one by of the sample holder thermocouple (TSample). As the heat transfers from the hot body (furnace heater) to “cold” body (sample) there is always a gradient of temperature between the furnace and the sample holder. As the thermocouple of the sample holder is placed close to sample the actual temperature of the sample is that measured by the sample holder thermocouple. So, in order that the sample reaches the setpoint temperature of 700 °C the furnace controlling algorithm adjusts the setpoint temperature to a higher setpoint temperature so that the sample temperature reaches 700 °C.

Can I control manually the HTF-1100?

Yes, it is possible to control manually the HTF-1100 furnace by setting the setpoint temperature directly on the Watlow controller at the front panel of the furnace. If you have a Bio-Logic potentiostat the sample’s temperature can be acquired through Analog In1 of the potentiostat. You can use a multimeter with thermocouple function to establish the linear relation between sample temperature and voltage to set in the “External Devices” tab window of Analog In1.

I performed impedance measurement at various temperatures. The temperatures displayed on the impedance plots are the setpoint temperatures. How can I access to the actual temperature of the sample at which the measurement has been performed?

You can access to the sample’s actual temperature at which the impedance measurement has been performed by selecting “Data” tab in the graphic window of MT-Lab® software and then select “sample temperature” column.

How can I access to the coordinates (frequency, phase, etc) of the measured points on an impedance diagram?

You can access to the coordinates of the measured points by clicking on “Data view”. A data view window is displayed. In case of multi- temperature graphs, select the graph and the impedance representation and then click on the point you want to display the coordinates. “Data view” is disabled during data acquisition.

How can I avoid temperature overshoot on the furnace and the sample temperature plot?

In order to reduce the overshoot observed on the temperature plot, we recommend to reduce the temperature ramp set in MT-Lab software. In MT-Lab software it is possible to lower the temperature ramp down 0.1 °C/min. Also, check that the sample holder thermocouple is well placed in its corresponding hole under the sample.

 

My sample is glued to the platinium discs of the HTSH-1100. How can I procced to remove the sample from the HTSH-1100 without broking the platinium wires?

In order to remove a glued sample to one or both platinium discs of the HTSH-1100 sample holder please proceed as follows:

– loosen the two bottom nuts to relax springs

– Gently raise the upper electrode. If you feel a resistance to discs opening this means that the sample is glued to platinum discs.

– Shake carefully the ring holding the upper Pt disc

– Use a cutter to separate the upper Pt disc from the sample. If the sample is still glued use a hot gun to blow hot air on DUT to facilitate its dismounting.

– Use a tweezer to remove the DUT from the HTSH-1100.

When can I use the Quartz tube with the HTSH-1100?

The quartz tube is only dedicated to tests under controlled environments (Inert or active gases). It is recommended to not use it if you do not controlled atmosphere.

Which connection mode do I need for connecting the HTSH-1100 to the MTZ-35 impedance analyzer?

It is recommended to use the “real two-terminal” connection to connect the HTSH-1100 to MTZ-35. This connection mode allows the MTZ-35 to reach very high frequencies. If the expected measured impedance is too low (lower than 1 Ohm), the four-point connection mode is recommended.

I cannot obtain a smooth and uniform sample’s surface. So can I test a sample with a rough and non-uniform surface with the HTSH-1100?

Yes, you can “smooth” the surface of your sample by depositing a conducting past on both side of the sample. The conducting past could be a silver, carbon, gold or platinium past. This method is not compatible with high porous sample (or pellet).

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