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SAFETY INFORMATION and OPERATING PROCEDURE

MASTER ALLOY CASTING

College/Dept: COEN Building/Room: HML 103

Laboratory Name: Magnetic Materials Lab Revision: 1

Approval

Authored by:

Doug Kellis (Research Engineer)

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Name, Title Signature Date

Reviewed and Approved by:

Peter Müllner (Principal Investigator)

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Name, Title Signature Date

Procedure Type Process/Protocol Chemical Hazard Class

Brief OverviewThis SOP describes the proper operation of the Master Alloy Casting process located in HML 103

ScopeFor use as a reference when casting master alloys

Potential Hazards Chemical Thermal Hydraulic Electrical Slip/Trip Biological

Mechanical Radiation Pneumatic Fire Fall Other

Hazard Specifics: Thermal Radiation, High Vacuum, Pressure

Engineering Controls (EC) Fume hood Biosafety Cabinet Other Local Exhaust Shielding Other

EC Specifics:

Certification of Hazard Assessment 1


Training Requirements – except for classroom lab safety, must be completed prior to performing the procedure

Classroom Laboratory Safety Radiation Worker

Online Safety Topics (specify): Gas Handling, Thermal Radiation, Chemical Safety

Lab/Work Group Specific Training (specify): General Lab Safety Tests

Other (specify): Operator Test

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Personal Protective Equipment (PPE) Safety glasses Safety goggles Face shield & safety glasses Face shield & safety goggles

Lab coat Apron Tyvek suit Tyvek sleeves

Gloves Leg coverings Hard hat Hearing protection

Respirator Shoes Fall protection Other

PPE Description: Nitrile gloves should be used when handling pure elements

Equipment, Materials, Supplies, & Facility RequirementsQuartz Tubes: Technical Glass Services Inc 108 W 31st Street Boise, ID 83714 208-426-8775Order Specs: 38mm OD x 35mm ID x 294mm long; closed one end with three Maria’s placed 175mm up from the closed end

Alumina Crucibles: Coorstek 303-277-4564Order Specs: Part # 66457-C-4.00: 31.75mm OD x 25.40mm ID x 101.6mm long; closed one end

Handling, Work Area & Storage Requirements Keep area clean and free of debris, do not re-use alumina crucibles

Spill, First Aid & Incident Requirements Report incidents to Dr. Peter Müllner (426-5136), Dick Sevier (426-1022), Matt Lundgren (426-3906), and fill out incident report form.

Decontamination & Waste Disposal Place used crucibles in broken glass container

Additional Safety Information Review of applicable safety references such as material safety data sheets to ensure appropriate protective measures, spill supplies, and first aid procedures.

References Pfeiffer Turbo Pump manual, Reitel Operators manual

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Procedure

REQUIRED EC & PPE*

Use of nitrile gloves, face shield, and darkened safety glasses required

* Applicable to all steps and substeps unless otherwise noted.

SYSTEM DESCRIPTION

The Master Alloy Casting system uses a multi-step process to produce an alloy. The first process evacuates the system and purges in an inert gas. The second process melts the constituent elements together to form the alloy. The main components of the system are:

1. Inert Gas Supply Systema. Gas Cylindersb. Restek Oxygen Getterc. Gas Control Valvesd. Gas Pressure Controller

2. Quartz tube/Crucible/Valve Assembly3. Reitel Induction Furnace4. LabView Control Program

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(1b)(1a)

(1c)(1d)


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(2) (3)

(4)


OPERATING STEPS

1. Quartz Tube and Crucible

a. Place constituent elements in Crucible.

b. Place the Crucible in Quartz Tubea. Quartz Tube must be at an angle so Crucible material will

not spill out of Crucible.

c. Gently slide Crucible to bottom of Quartz Tube.

d. Insert Quart Tube into Hybrid Adapter.

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e. Tighten the Collar on the Hybrid Adapter.

f. Open the Butterfly Valve. (This is a ¼ turn valve)

g. Open the Bellows Valve. (Turn the valve 1-3 turns)

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2. Evacuating the System

a. Click on the Manual Control icon on the desktop.

b. The Manual Control panel will appear.

c. Press the Turbo Pump Valve Open/Close button. (The green light on the button will glow when the valve is open)

d. Press the Start/Stop Pump button. (The green light on the button will glow when the pump is running)

e. Allow the system to run until the Pressure is ~ 3.xx E4 mbar.

Certification of Hazard Assessment 8


f. Set the Pressure Controller SetPoint to 5.

g. Press the Turbo Pump Valve Open/Close button.(The green light on the button will be off when the valve is closed)

h. Press the Argon Valve Open/Close button. (The green light on the button will glow when the valve is open)

i. Allow the system to run until the Pressure is ~ 5.00 E+2 mbar.

j. Press the Argon Valve Open/Close button.(The green light on the button will be off when the valve is closed)

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k. Close the Butterfly Valve.

l. Close the Bellows Valve.(Turn the valve until it seats, then apply light pressure to ensure valve is seated)

m. Press the Start/Stop Pump button.(The green light on the button will be off when the pump is off)

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3. Producing an Alloy

n. Loosen the Clamp at the base of the Bellows Valve.

o. Carefully remove the Clamp while holding the Bellows Valve.

p. Place the Vacuum Port Cover over the open Vacuum Port.

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q. Slide the Quartz Tube/Crucible/Bellows Valve Assembly onto the Assembly Rod holder.

r. Guide the Quartz Tube into the Induction Coil in the Reitel Furnace.

s. Align the Quartz Tube such that it is centered in the Induction Coil.

t. Allow the Quartz Tube/Crucible/Bellows Valve Assembly to seat against the Assembly Stop.

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u. Close the Locking Lever on the Reitel Furnace ensuring that the Magnet is located close to but Not touching the Safety Switch.

v. Turn the Power Switch to the Reitel Furnace to the On position. (Green LED should glow steady)

w. Turn the Main System Knob to Position 1.

x. Turn the Heater Knob to 10.

y. Heat the Quartz Tube/Crucible/Bellows Valve Assembly until the Crucible is glowing. Allow the Alloy to heat for approximately 2-3 minutes.

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z. Turn the Heater Knob to 0.

aa. Turn the Main System Knob to 0.

bb. Allow the Crucible to cool for at least 30 minutes before removing it from the Induction Coil.

cc. Lift the entire Quartz Tube/Crucible/Bellows Valve Assembly up and out of the Reitel Furnace.

dd. Swing the Quartz Tube/Crucible/Bellows Valve Assembly to the right, slide the Quartz Tube/Crucible/Bellows Valve Assembly back down until it comes to rest against the Assembly Stop.

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ee. Open the Bellows Valve. (Turn the valve 1-3 turns)

ff. Loosen the Collar on the Hybrid Adapter. (Hold the Quartz Tube while doing this)

gg. Slide the Quartz Tube out of the Hybrid Adapter and remove the Crucible.

hh. Close the Bellows Valve.(Turn the valve until it seats, then apply light pressure to ensure valve is seated)

ii. Remove the Vacuum Port Cover and set the Bellows Valve back onto the Vacuum Tube. Reassemble the Clamp and recover the Hybrid Adapter with the plastic bag.

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jj. Turn the Power Switch to the Reitel Furnace to the Off position. (Green LED should not be lit)

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