NANOE Zetasinter User manual

ZetaMix System®
Fevrier 2022
Thank you for purchasing the Zetasinter furnace. To avoid any misuse and damage, please read the operations manual
carefully before using.
NANOE SAS
C O N T A C T @ N A N O E . C O M |
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B A L L AIN V IL L I E R S
F R A N C E
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High Temperature tube furnace
Operations Manual

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Zetasinter System®
Content
1. Furnace Description..................................................................................................................................... 3
2. Technical Specifications............................................................................................................................... 3
3. Safety........................................................................................................................................................... 4
a. Intended use
b. Assembling
c. Operation
d. Maintenance
4. Assembling................................................................................................................................................... 7
5. Temperature controller............................................................................................................................... 9
6. Alumina tube and refractory blocks.......................................................................................................... 14
7. Vacuum pump & flowmeter....................................................................................................................... 19
8. Bubbler …………………………………………………………………………………………………………………..…………………………..…..…21
9. MoSi2 Heating elements……………………………………………………………………………………………………………………………. 22
10. Troubleshooting....................................................................................................................................... 23
11. Electrical schematic diagram.................................................................................................................... 25
12. Quick start procedure .............................................................................................................................. 26
13. EU Declaration of conformity (No 2018-11-a) ......................................................................................... 27

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Zetasinter System®
1. Furnace Description
The Zetasinter Tubular Furnace is a tubular furnace using MoSi2 heating elements and a high purity alumina
tube, working temperatures are between 800℃and 1550℃. Zetamix printed parts must be placed inside the
tube sealed with flanges. Depending on the material, they can be sintered in an ambient or inert
atmosphere.
2. Technical Specifications
Heating Power
3.5 kW
Voltage / Frequency / Current
220V / 50Hz / 32A
Maximum temp.
1600°C
Working Temp.
1550°C
Suggested heating rate
≤3°C/min
Temperature controller accuracy
±1°C
Thermocouple
B type
Heating elements
6 x U type MoSi2
Size
860x605x1120mm –112 kg
Chamber size
Ø90x100mm

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Zetasinter System®
3. Safety
a. Intended use
Only parts printed with Zetamix by Nanoe® filaments can be heat treated in Zetasinter. Reference names of
Zetasinter by Nanoe® filaments are:
- Zetamix H13 Steel®
- Zetamix H13 Steel®
- Zetamix White Zirconia®
- Zetamix Black Zirconia®
- Zetamix Alumine®
Installation must be done according the Zetasinter facility guide.
Installation, use and maintenance must be done according to this operation manual.
b. Assembling
Assembling must be done according to this operation manual.
Only the vacuum pump can be connected to the socket on the side of the furnace body.
Danger due to electrical Current.
During installation and maintenance
work, the electric supply to the furnace
must be switched off.
Work on electrical equipments may only
be performed by qualified personnel.
The set-up instructions and safety
regulations must be observed,
otherwise the furnace will be deemed
to have been used incorrectly,
effectively cancelling any claims
against Nanoe.

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Zetasinter System®
c. Operation
Temperature controller
For each material reference, the heat program must be defined by the operator according to guidelines provided
by Nanoe (www.zetamix.fr).
The maximum safety temperature is set at 1600°C. Above, the temperature controller automatically stops the heat
treatment.
The recommended maximum working temperature is 1550°C.
Heating and cooling rates may not exceed 3oC/min (except emergency stop).
Do not turn off the power supply of the equipment if the furnace temperature is above 500°C.
After replacing the temperature controller, its settings must be adjusted before use.
Alumina tube and refractory blocks
Put the refractory blocks on both sides of the tube before starting a heating cycle and wait until the furnace
temperature drops to room temperature (<100°C) before removing them.
Do not touch the inner or outer surface of the furnace during or immediately after use.
Do not place any objects on the furnace body.
Vacuum pump
Check the oil level before use.
Gas supply
Working at a positive relative pressure is not recommended for the alumina tube. The relative pressure must not
exceed 0.2 bar (0.02 MPa). Inlet and outlet flanges must remain open during the heat treatment. Switch off the
furnace (hold or stop conditions) if the pressure exceeds 0.2 bar (0.02 MPa) and/or the bubbler is not bubbling.
Positive relative pressure is not
recommended for this product. The
relative gas supply pressure should not
exceed 0.2 bar (0.02 MPa) and the
flanges should be properly adjusted.
Hot surfaces, danger of burning.
You may not always realize that surfaces,
such as the furnace walls, tube and
crucible are hot. Do not touch the
surface.

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Zetasinter System®
d. Maintenance
The power supply must be switched off before any maintenance work.
Inert gases such as argon are dangerous
because of the risk of asphyxiation.
The working area must be ventilated
using an appropriate ventilation system.
The use of an oxygen monitor is
recommended.
Danger due to electrical current.
During installation and maintenance
work, the electric supply to the furnace
must be switched off.
Work on the electrical equipment may
only be performed by qualified
personnel.

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Zetasinter System®
4. Assembling
-Install the furnace according to the facility guide.
-Remove the plastic cover from the heating elements under the top cover (remove the screws to do
this).
-Install the alumina tube. Put the refractory blocks on both sides of the tube (cf. Alumina tube
chapter).
-Close the circuit breaker, turn on the power →the green light comes on and the cooling fan starts to
work.
-Turn the “lock”button clockwise →the temperature control unit is now switched on.
-Press the “Turn On”button (green light is now on).
Danger due to electrical current.
During installation and maintenance
work, the electric supply to the furnace
must be switched off.
Work on the electrical equipment may
only be performed by qualified
personnel.

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Zetasinter System®
Temprature controller
Turn ON
Turn ON
Lock
Cycle Left, Down, Up arrows
Selection screen
T/time screen
-For the first heating, the furnace chamber must be “baked”for 2 hours at 300℃. Using the
temperature controller, program and run the "baking" cycle (cf. Temperature controller chapter):
(C01=50; t01=85; C02=300; t02=120; C03=300; t03=65; C04=100; t04=-121)
-For the first high temperature heating (above 400°C), heating element must be “passivated”for 2
hours at 1200°C (cf. heating element chapter). Using the temperature controller, program and run
the "passivation" cycle:
(C01=50 ; t01=385 ; C02=1200; t02=120; C03=1200; t03=365; C04=100; t04=-121)
-Install the vacuum pump and the flowmeter (cf. Vacuum pump & flowmeter chapter).
-Install the bubbler (cf. Bubbler chapter).

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Zetasinter System®
5. Temperature controller
Heating program setting
Program state symbols
Stop state
When you turn on the “Lock”, the temperature controller displays the model and version. After a few
seconds, it switches to the off-state.
-PV : “TC temperature”(50°C at room temperature).
-SV : “StoP” is alternately displayed on the lower window.
①Process value (Thermo couple temperature °C)
（P V）
②Setting value (temperature °C- Program state*)
（S V）
③Setting key (confirm KEY)
④Data shift key (and program setup entry)
⑤Data reduction key (and program RUN/HOLD）
⑥Data add key (and program STOP）
⑦Function indicator :
-PRG controller in running state
-OP1 power output
-OP2 power output level
-COM Communication interface
-Other lamps not use

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Zetasinter System®
Heating program setting
①From stop state, Press to go to the setup program state.
②The set points of the step StEPXX are displayed (C XX temperature in °C, and t XX time in min).
③Press , and to modify the value.
④Press to move to the next parameter. The program parameters are displayed in the following order:
setpoint1, time1, setpoint2, time2.
-Press and hold to return to the previous setting. The program step can be changed at any time,
even if the program is running.
⑤Set t××= -121 to indicate the end of the program (automatic switch-off).

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Zetasinter System®
⑥Press and simultaneously to exit the settings. If no key is pressed within 25 seconds, it also
exits to stop state.
Example:

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Zetasinter System®
Specific settings:
Time Setting
Heating programs saving

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Zetasinter System®
Run/Hold states
Run state:
In Stop state, press and hold until the SV window displays the “run” symbol. The controller runs the
defined program.
Hold state:

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Zetasinter System®
In Run state, press and hold until the SV window displays the “HoLd” symbol. Controller holds the
given temperature and stop the timer.
In Hold state, press the until the SV window displays the “run” symbol. Controller starts running
again.
Step number and timer:
In Run or Hold states, press to display the current step number and timer (PV: current step time
setting and SV: current step elapsed time).
Return to Stop state:
In Run or Hold states, press, and hold until the SV window displays the “StoP” symbol. The controller
will stop (free cooling), the timer will be reset, and the step number will be set to 1.
6. Alumina tube and refractory blocks
Alumina tube
①Switch off the power supply.

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Zetasinter System®
②Install the heat shields.
③Carefully insert the tube into the furnace, keep it straight to avoid breaking the heating elements. Keep
an equal length of tube at both ends of the furnace.
④Install the tube holders.
Wrap the threads with PTFE tape and connect the pressure gauge and intake valves to the flanges:
The installation of the sealing flanges is shown in the figure below:
Right: Inlet flange (OD 6mm connection to the gas
supply)
Left: Outlet flange (OD 10mm connection to the vacuum
pump or to the bubbler)

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Zetasinter System®
Install the right flange (inlet flange):
1) 2)
3) 4)
5)
Install the left flange (outlet flange) ：

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Zetasinter System®
1) 2)
3) 4)
5) 6)
7)
Adjust the position of the tube holders under the flanges, they must be in contact with the flanges.
Use: refractory blocks and alumina plate

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Zetasinter System®
-Install the four refractory blocks (Ø85x90mm) and the alumina plate (100x75mm →possibility of
using 2)
-Two refractory blocks must be placed almost in contact with the crucible as shown in the figure
below. It is recommended to use marks on the crucible hook at 36, 45 and 55 cm.
-If the refractory blocks are not positioned correctly, this can lead to tube failure.
Maintenance
After every heat treatment:
-Clean the binder residues in the outlet flange with a degreaser. Use a
bottle brush to clean the outlet valve. Please note that only
refractory blocks are required to debind/sinter Zetamix ceramics. No
need to put and close the flanges.

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Zetasinter System®
After five heat treatment:
-If the refractory blocks and the alumina plate are black due to binder residue. Program and run an
“cleaning cycle”under ambient atmosphere (inlet and outlet valves open):
(C01=50; t01=485; C02=1500; t02=120; C03=1500; t03=467; C04=100; t04=-121)

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Zetasinter System®
7. Vacuum pump & flowmeter
Vacuum pump
①Unscrew the blue vacuum pump cap and inject the appropriate amount of oil. Put back the vacuum
pump cap without (without the small black cover).
②Plug the vacuum pump into the socket on the side of the furnace body.
③Connect the vacuum pump to the outlet flange using the Ø10mm flexible air hose.
1) 2)
.
Flowmeter
①Install the flowmeter on its holder.
②Connect its outlet (upwards) to the inlet flange with the Ø6mm flexible air hose.
③Connect its inlet (downwards) to the 0.2 bar (0.02MPa) gas supply (1/8 NPT F).
1) 2) 3)
Use: Flushing
-Close the valves and the flowmeter.
-Turn on the pump.
-Open the outlet valve.
-Wait till the tube pressure is under -0.9 bar (-0.09 MPa).
-Close the outlet valve.