Differences

This shows you the differences between two versions of the page.

--- lindberg_blue_tube_oven [2022/11/24 09:08] – [Cool down and finish] scholma
+++ lindberg_blue_tube_oven [2023/03/31 09:20] (current) – [Oxygen and Argong tube oven annealing] scholma
@@ Line 1: / Line 1: @@
-====== Tube oven annealing ======
+====== Oxygen and Argon tube oven annealing ======
-The tube oven has a temperature range of xx-xxxx °C and can fit 1 inch diameter tubes. Temperature regulation is done by a Lindberg/Blue UP150 controller.
+The tube oven has a temperature range of up to 1100 °C and can fit 26mm diameter tubes. Temperature regulation is done by a Lindberg/Blue UP150 controller. \\
+Oxygen and Argon can be connected separately or mixed. Setting the gas flows is done via a needle valve separately for O2 and Ar.
@@ Line 7: / Line 7: @@
   * read safety notes below
   * Keep the components clean and do not use tubes that are not assigned to you
+  * wear gloves
   * Make sure to mark or label your tube if you wish to keep it clean and keep it in the cupboard
   * Indicate whether samples are loaded or not
@@ Line 13: / Line 14: @@
 ===== Tube specifications =====
-Outer diameter: 25mm or 1 inch (25.4mm)\\
+Outer diameter: 26mm \\
-Length: between xxcm and xxcm
+Length: between 55cm and 65cm
-Operating temperatures:
+Operating temperatures of boat and tube material:
   * Pyrex: 500°C (greenish color when viewing the edges)
   * Quartz: 1000°C
   * Al2O3: 1700°C
-====== Safety ======
-Most important safety points are:
-  * high temperature
-  * pressurized gas cylinders
 ==== High temperature safety ====
-Always lock the oven when a process is running.
+  * Always lock the oven when a process is running.
-Let process cool down to 50°C before handling any components.
+  * Let process cool down to 50°C before handling any components.
-No organic solvents on the table when a process is running.
+  * No organic solvents on the table when a process is running.
-Work with clean tubes
+  * Work with clean tubes
 ==== Pressurized gas cylinders safety====
-Do not attempt to change cylinders or connected equipment, always consult with a technician.
+Do not attempt to change cylinders or connected equipment, **always** consult with a technician.
 ===== Setting up and starting the process =====
   * check that your tube and sample boat have a higher operating temperature specified than your process temperature
+  * load sample and connect tube adaptors
+  * double check pressure reducers on the cylinders are closed
+  * open cylinder(s) you need (make sure there is enough oxygen for you proces)
+  * set 1 bar on secondary pressure gauge
+  * set desired flow rate with needle valve for both gasses separately.
+  * setup heater program and start (see below on how to use the temperature controller)
 ===== Cool down and finish =====
       * if you operated in single setpoint mode: turn off oven manually
-      * wait until oven temp is below 50°C before taking out the sample
+      * wait until oven temp is below 50°C
-      * close cylinder, keep flow until pressure on primary and secundary pressure gauges are 0.
+      * close cylinders with the angle key on the top of the cylinder, keep flow on until pressure on primary and secondary pressure gauges is 0. You can increase flow a bit if this takes a long time.
-      * close reducer and needle valve
+      * close manual valves, needle valves and pressure reducers
-      * take out sample and put aluminium foil on parts to keep them clean
+      * take out sample and put a tube back to keep everything clean.
 ==== Using the UP150 temperature controller ====
+{{::temperature_program.jpg?nolink&400|Temperature program with multiple segments}}
+A typical program for us will have three segments, a ramp-up, a dwell and ramp-down segment.\\
+In the ramp-up segment you specify the desired temperature and how fast you want to reach this temperature (do not heat to quickly).\\
+In the dwell segment you set the time how long you want to stay at the desired temperature in hours.\\
+In the ramp-down segment you specify the desired temperature and how fast you want to reach this temperature, since we don't have active cooling, the cooldown rate cannot be made faster.
+=== changing ramp-up segment ===
+  * hold set/ent button for 3 sec to go into the menu
+  * with set/ent button navigate to PrG
+  * set PrG to 1 with ▲
+  * set/ent button to confirm and enter the program
+  * with set/ent button navigate to SP1
+  * change desired temperature with ▼ and ▲, set/ent button to confirm
+  * change Tn1 with ▼ and ▲ (displayed in hours)
+  * hold set/ent button 3 sec to go back to main display
+Start program: hold ▼ for 3sec
+Stop program: hold ▲ for 3sec
+{{:lindberg-blue_up150_temperature_controller_manual.pdf|Manual UP150 controller}}
-You can operate the temperature controller in two modes:
-  * single setpoint mode: the controller will go to the desired temperature and maintain the temperature indefinitely, you have to turn the oven off manually
-  * programming mode: the user can enter a series of setpoint and time values, the controller will follow the sequence.
-[[lindberg_blue_tube_oven|Manual UP150 controller]]