Advanced High Pressure Oxygen Furnace A-HSO

Advanced high pressure oxygen furnace A-HSOA-HSO: Quenching and Gas Management Upgrades

  • Annealing oxide rods at up to 1200 °C
  • Quenching metastable phases at high pressures of 200 bar
  • Adjust and manipulate stable and flowing gas mixtures

Some material states with highly interesting properties are only stable under high temperatures and high pressure atmospheres with a precisely defined partial pressure of oxygen. During cooling and releasing the pressure to ambient conditions or changing the oxygen content in the atmosphere, these elusive states often decompose, making the analysis of their physical properties almost impossible. By quenching the sample within milliseconds under defined high pressure atmospheres, the metastable material states freeze and their properties remain under ambient conditions. Advanced HSO: Quenching and Gas Management Upgrades Up to now, extensive research on such materials was impossible due to the absence of a suitable device allowing the synthesis and quenching of the sample under high pressure conditions. With the “Quenching and Gas Management Upgrade” to our High Pressure Oxygen Furnace HSO we create an instrument, which for the first time combines the possibility to rapidly quench the sample, treat the sample under high temperatures, enable high gas pressures and have full control of oxygen content in the process atmosphere between 0 and 100 %.

Going beyond standard HSO parameters, the total pressure can be set up to 200 bar and the temperature up to 1200 °C. While the standard HSO furnace is designed to operate horizontally, the A-HSO is set up vertically. The sample is mounted in a hanging position within the heating zone of the process chamber. When the sample is ready to be quenched, the mounting system is released and the sample drops into a quenching chamber, which is located underneath. This chamber is designed to be filled with water, but many other liquid or solid quenching media can be used. The release of the sample mounting system and the drop of the sample can be triggered manually or automatically, e.g. after a certain amount of time or other measured value thresholds. The lower chamber is filled with the same atmosphere as the process chamber and is valved off with a rapidly operating automatic gate valve. During the process, the atmosphere around the sample can be freely adjusted in terms of total pressure, gas mixture and individual gas flow rates. Typically, the sample chamber is filled with static or dynamic gas of O2/Ar mixtures. The elaborated gas management system includes precise mass flow controllers for each gas and allows in-situ manual or automatic changes to the process atmosphere at anytime of the process. A precise thermocouple element sits near the sample, a set of additional thermocouples monitors the furnace temperature in different places. All experimental parameters such furnace and sample temperatures, gas pressure, mixture and flow aswell as the release of the sample mounting system are controlled by a build-in computer. A comfortable software application combines all relevant system information and process adjustments in one graphical user interface unit.

 

Main components

Figure: Sketch of A-HSO main components and quenching procedure. Left: A-HSO with sample mounted in heating position. Right: A-HSO with released sample mounting system, sample droped through the open valve into the quenching liqiud.

 

Technical details

Atmosphere
• Process chamber gas:  oxygen and argon (pure and in any mixture)
• Many other gases possible on request
• Pressure: 1 to 200 bar
• Automatically controlled gas flow up to 1 l/min (higher flow rates possible on request)
• Each gas adjustable independently with an individual mass flow controller
• Precise oxygen content measurement system
• Heating elements chamber gas: argon (other inert gases possible on request, e.g. He, N2 etc.)
• Automatized pressure control while heating and cooling

Heating
• Specialized resistive heating elements
• Long life span due to protective environment
• Maintenance-free operation
• Maximum temperature: 1200 °C, higher temperatures possible on request

Process chamber
• Dimensions: diameter 25 mm, heating zone length 200 mm
• Chamber material: non-reactive material withstanding high-pressure oxygen under high temperatures
• Precise thermocouple element for permanent temperature monitoring

Outer pressure tube
• Water-cooled metal casing
• No material fatigue due to low temperatures and non-reactive environments

Process control
• Build-in computer unit for all controlling purposes
• All system parameters are controllable and adjustable via a comfortable GUI on a build-in touchscreen
• Fully automatic or manual operation
• Power ramp functions with several temperature steps and heating/cooling rates adjustable
• Pressure pump functions with several pressure steps and rates adjustable  
• Permanent data logging function

Quenching Upgrade
• Sample release system, automatically or manually triggered at any time
• Lower quenching chamber filled with water or other quenching media
• Lower chamber separated by an automatically operated gate valve

Required laboratory connections
• 210 bar oxygen and argon gas supply with constant pressure rate
• Energy supply: AC single phase 220-240 V
• Cooling water with approx. 20 °C,  pressure up to 3 bar, min. 4 liter/min, 4000 W cooling power

 

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