final list of metal alkoxides ordered + all MSDS...

Robert Huang roberth at quswami.com
Fri Apr 30 13:46:30 PDT 2010


 Hi Mary,

After further literature search, I have decided not to do an anneal after immersion of my wafers in these metal alkoxide solutions.  To be clear, here are the details of the processing I intend to do, including the full set of steps after the metal deposition via these liquid solutions:


1)      "Dip" full 4" wafers into these metal alkoxide/solvent solutions at wbsolvent.  I plan to use the hotplates and my own glassware to heat the solutions to 70C.  The deposition times will be on the order of minutes, and I'll stay with the wafers/solutions at all times throughout processing.

2)      Removal from solution, then rinse at wbsolvent with appropriate solvent (either propanol or methanol), followed by N2 dry

3)      DI water rinse at wbgeneral followed by N2 dry

4)      Metal deposition on metallica

5)      Metal deposition on innotec

That's it.  Let me know if there are any other concerns.  At the moment, I plan to process wafers through this sequence in mid-May timeframe.

Regards,

Robert
________________________________
From: Mary Tang [mtang at stanford.edu]
Sent: Monday, April 26, 2010 8:18 AM
To: Robert Huang
Cc: specmat at snf.stanford.edu
Subject: Re: final list of metal alkoxides ordered + all MSDS...
Thanks Robert --

Just a few questions:  are there environmental constraints on your anneal?  (Inert gas?  Temperature control?  Cleanliness -- where do your wafers go afterwards?)

Also, is there a recommended hot plate pre-treatment before the anneal?

And how long is your anneal?

fga2 is one option.  We have a Thermolyne muffle furnace outside the lab (no inert gas, but faster ramp/dwell/cool.)   It might be a good to try to minimize organics off-gasing with a prebake, which is often done for spin-on products.


Mary

Robert Huang wrote:
Hi Mary, SNF Specmat Committee,

I decided to order all the chemicals from Sigma Aldrich, including the anhydrous methanol and propanol that I will be using.  Below is the full list of what I'll be using, and I'm attaching all MSDS sheets here so that you have them in a single location.
Item #

Description

# of Units

341436

Tetramethyl orthosilicate - 25g

1

333948

Zirconium butoxide - 100ml

1

667943

Hafnium n-butoxide - 5g

2

201073

Aluminum tri-sec butoxide - 5g

1

322415

Dry Methanol - 100ml

1

278475

Dry2 Propanol - 100ml

3


Regards,

Robert

-----Original Message-----
From: Robert Huang
Sent: Monday, April 19, 2010 2:52 PM
To: 'Mary Tang'
Cc: specmat at snf.stanford.edu<mailto:specmat at snf.stanford.edu>
Subject: RE: additional material...RE: Addition to request to use aluminum tri-sec butoxide in SNF...

Hi Mary,

I have obtained access to an anaerobic glovebox on-campus at Stanford (also in CIS).  After preparing the solutions in the glovebox, I will transport the chemicals using the transport containers in the stockroom, and the solutions will remain in sealed containers during transport.  Once I'm in SNF, I will then be working at wbsolvent to immerse my wafers in solution heating the solution to 60-70C.  Do you see any other issues or concerns?  If not, I plan to go ahead and order the chemicals.

One final question, if I want to then anneal the wafers up to say 450C, would the specmat committee allow me to put the wafers in the FGA tube?  If not the FGA tube, any other appropriate equipment to do the anneal?

Regards,

Robert

-----Original Message-----
From: Mary Tang [mailto:mtang at stanford.edu]
Sent: Thursday, March 11, 2010 11:14 AM
To: Robert Huang
Cc: specmat at snf.stanford.edu<mailto:specmat at snf.stanford.edu>
Subject: Re: additional material...RE: Addition to request to use aluminum tri-sec butoxide in SNF...

Hi Robert --

Thanks!  The protocol describes preparation of the solutions in dry-IPA
under anaerobic glovebox conditions.  I'm afraid we do not have a
glovebox here at SNF -- were you planning to make up your solutions
here?   I'm also not sure how water/air reactive these chemicals are --
the MSDS say that they can form possibly explosive mixtures with water
-- but then, the MSDS for octadecyl trichlorosilane (OTS) says the same
and this is used a lot in the lab.  I suspect the chemicals you have are
similar, but you should check on this with the supplier.  (OTS is
moisture and air sensitive, but basically means that when you let it sit
around for a few hours, it turns into useless sand, but if you work
quickly, you can get a good surface coating down.)

So again, please check with your supplier on recommendations for
handling and using these chemicals.  We can't provide a glovebox here,
but you may not need one.  Our primary concern is safety (if these are,
indeed, explosive, then these are a definite no).  The secondary concern
is whether air/moisture exposure will adversely affect your experiment.
Please let us know what your supplier or other knowledgeable source
recommends.


Mary

Robert Huang wrote:
> Dear SNF Spec Mat committee:
>
> Attached is a paper which provides more details on how I plan to use
> these chemicals.  Look at the 1st paragraph in "Experimental Section"
> on p. 476 as well as the paragraph on p. 477 that starts "After
> sintering...".
>
> Regards,
>
> Robert
> ------------------------------------------------------------------------
> *From:* Robert Huang
> *Sent:* Monday, March 08, 2010 12:46 PM
> *To:* specmat at snf.stanford.edu<mailto:specmat at snf.stanford.edu>
> *Subject:* Addition to request to use aluminum tri-sec butoxide in SNF...
>
> Dear SNF Spec Mat committee:
>
>
>
> In addition to using aluminum tri-sec butoxide from Sigma-Aldrich, I'd
> like to use the following chemicals from Strem (links to Strem website
> are given and MSDS sheets attached):
>
>
>
> 1)      Aluminum s-butoxide - http://www.strem.com/catalog/v/93-1308/
> (composition is actually the same as aluminum tri-sec butoxide from
> Sigma Aldrich, my original request)
>
> 2)      Hafnium t-butoxide - http://www.strem.com/catalog/v/72-5800/
>
> 3)      Tetramethoxysilane - http://www.strem.com/catalog/v/93-1459/
>
> 4)      Zirconium n-butoxide - http://www.strem.com/catalog/v/93-4003/
>
>
>
> As with the aluminum tri-sec butoxide, I would be diluting these
> materials in dry2-propanol (or methanol) and dipping my 4" wafers into
> the solution.  Total solution will remain 100-200mL, just enough to
> immerse my wafers, and I will then process the wafers on innotec and
> metallica.
>
>
>
> Please review these chemicals as well and let me know if there are any
> concerns.
>
>
>
> Regards,
>
>
>
> Robert
>
>
>
> *From:* Robert Huang
> *Sent:* Friday, March 05, 2010 9:15 AM
> *To:* specmat at snf.stanford.edu<mailto:specmat at snf.stanford.edu>
> *Subject:* request to use aluminum tri-sec butoxide in SNF...
>
>
>
> Dear SNF Spec Mat committee:
>
>
>
> I would like to use a new chemical in SNF, aluminum tri-sec butoxide
> (99.99% trace metal basis), and would be obtaining 5-10mL in solution
> from Sigma-Aldrich.  Below is a link to their website on this material:
>
>
>
> http://www.sigmaaldrich.com/catalog/ProductDetail.do?lang=en&N4=511609|ALDRICH&N5=SEARCH_CONCAT_PNO|BRAND_KEY&F=SPEC
> <http://www.sigmaaldrich.com/catalog/ProductDetail.do?lang=en&N4=511609%7CALDRICH&N5=SEARCH_CONCAT_PNO%7CBRAND_KEY&F=SPEC><http://www.sigmaaldrich.com/catalog/ProductDetail.do?lang=en&N4=511609%7CALDRICH&N5=SEARCH_CONCAT_PNO%7CBRAND_KEY&F=SPEC>
>
>
>
> In addition, I'm attaching the MSDS sheet for this material.
>
>
>
> My intent is to dilute this material (comes in liquid form) in
> dry2-propanol, then dip my 4" wafers into the solution.  I presume
> this processing would need to be done at wbsolvent.  I plan to use
> 100-200mL of total solution in quartzware, basically whatever is the
> minimum amount needed that will allow me to immerse my wafers in the
> solution.  Afterwards I intend to process the wafers further on the
> innotec and metallica tools.
>
>
>
> Please let me know if there are any concerns or any special handling
> requirements.
>
>
>
> Regards,
>
>
>
> Robert Huang
>
> roberth at quswami.com<mailto:roberth at quswami.com> <mailto:roberth at quswami.com><mailto:roberth at quswami.com>
>
> 408-854-0450
>


--
Mary X. Tang, Ph.D.
Stanford Nanofabrication Facility
CIS Room 136, Mail Code 4070
Stanford, CA  94305
(650)723-9980
mtang at stanford.edu<mailto:mtang at stanford.edu>
http://snf.stanford.edu




--

Mary X. Tang, Ph.D.

Stanford Nanofabrication Facility

CIS Room 136, Mail Code 4070

Stanford, CA  94305

(650)723-9980

mtang at stanford.edu<mailto:mtang at stanford.edu>

http://snf.stanford.edu
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