SOP and procefure for vapor Silanation

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UCSB Lab-specific Chemical Hygiene Plan
Standard Operating Procedure:
Vapor deposition of silanes
(TRIDECAFLUORO-1,1,2,2-TETRAHYDROOCTYL)TRICHLOROSILANE
(C8H4Cl3F13Si)
or
N-DECYLTRICHLOROSILANE
(TRIDECAFLUORO-1,1,2,2-TETRAHYDROOCTYL)TRICHLOROSILANE (C8H4Cl3F13Si)
C8H4Cl3F13Si reacts with water to make hydrogen chloride. Do not inhale.
Handle only in fume hood.
Date of last revision to SOP: 26 May 2014
1. (TRIDECAFLUORO-1,1,2,2-TETRAHYDROOCTYL)TRICHLOROSILANE
(C8H4Cl3F13Si)
2. N-DECYLTRICHLOROSILANE
C8H4Cl3F13Si Safety Data Sheet
3. Approval Required
Users must undergo training before using this chemical.
4. Personal Protective Equipment
 Protective eyewear such as approved safety glasses, goggles required.
 Lab coat required.
 Rubber, neoprene, or nitrile gloves required.
5. Engineering/Ventilation Controls
 Only use in fume hood. Use on the open bench is prohibited.
 Only open in nitrogen atmosphere. Reacts with water vapor in the air.
6. Chemical Handling, Storage, Cleanup and Disposal Requirements
 Conditions to avoid: Combustible; avoid contact with heat, sparks or open flame.
 Incompatibility: Reacts with water and moisture in air, liberating hydrogen
chloride. Avoid contact with alcohols, acids, and oxidizers.
 Hazardous decomposition products: Organic acid vapors, hydrogen chloride, and
fluorinated organics.
 The vial must be stored in a completely sealed container. Visually examine for
leak before opening the outer container.
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Templates revised 9/2012
UCSB Lab-specific Chemical Hygiene Plan
 In case of spill: Cover spill with absorbent material. Transfer to a suitable container
for disposal. Report to EH&S for assistance.
 Disposal must be done through EH&S. No chemical wastes can go into the sewer
system, trash or be allowed to freely evaporate.
Chemical Vapor Deposition of tridecafluoro-1 1 2 2tetrahydrooctyl-1-trichlorosilane
Meinhart Lab Protocol, updated 4/18/2013
** This protocol involves a dangerous chemical, refer to the SOP and MSDS prior to
handling it **
*Do not perform this protocol if you have not been trained by an authorized user*
This protocol is intended for gas-phase monolayer deposition of a silane, to serve as a
counter-adhesion agent, for glass or silicon substrates. The chemical “tridecafluoro-1 1 2
2-tetrahydrooctyl-1-trichlorosilane” will be referred to as silane for the purposes of this
protocol. It can be deposited onto silicon and glass substrates. It will etch metal oxides
(e.g. alumina).
*The silane reacts with water vapor in air to create hazardous vapor. Do not handle
outside the fumehood. *
1. Put vacuum chamber in fume hood. Use only the vacuum chamber specified
for this procedure.
2. Optional: Place clean room wipe on top of the metal platform in the vacuum
chamber.
3. Make sure substrate is completely dry, and place it in the vacuum chamber,
with the side on which the monolayer will be deposited exposed.
4. Remove the vial of silane from its secondary container, and without opening
it, place it in the vacuum chamber.
5. Close the chamber with the bell.
6. Connect the house vacuum line to the vacuum chamber.
7. Pump down chamber to expel any water vapor from surfaces: about 1 minute
for a clean, flat, and dry substrate.
8. Seal chamber using the stopcock.
9. Connect N2 line to the vacuum chamber.
10. Start N2 flow, and allow bell to completely fill with N2.
11. With N2 continuing to flow, open the bell enough to reach with your hand the
vial of silane. The purpose of this is that no atmospheric air enters the
vacuum chamber.
12. ** With one hand holding open the bell, and the other holding the vial of
silane, carefully open the vial and place the open vial back into the vacuum
chamber, with the lid next to the now open vial in the vacuum chamber.**
13. Replace bell on vacuum chamber.
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Templates revised 9/12
UCSB Lab-specific Chemical Hygiene Plan
14. Turn off N2 supply.
15. Connect vacuum chamber with vacuum line, and open the vacuum line.
16. Allow vacuum chamber to be evacuated of the N2 atmosphere, until hissing
stops, about 2-3 minutes.
17. Close stopcock so that the silane atmosphere does not escape through the
vacuum line.
18. Allow to sit for between 30 minutes and 1 hour, but no longer than one hour.
19. Turn on vacuum and open stopcock to remove the silane atmosphere.
20. Close stopcock, turn off vacuum, and connect N2 line to the chamber.
21. Open stopcock and turn on N2 flow slightly.
22. Once N2 atmosphere with positive pressure is established increase the N2
flow to prevent atmospheric air from entering the chamber and lift bell slightly
away from vacuum chamber w/ one hand, and with the other hand recap the
vial while still under the bell.
23. Place the silane vial in the secondary contained and make sure it’s sealed
tightly.
24. Remove sample and put away materials as appropriate.
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Templates revised 9/12
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