New SNF Chemical (6 of 6): n-propyl zirconate

[Bree Sharratt]

Hello Mary and others,

First, to clarify: all the materials are in liquid form.

About the heat treatment after spin-coating:  I am hoping not to have 
to heat treat but to just "babysit" them under the exhaust long enough 
to allow the solvent to disperse so that I avoid any changes in the 
film before I continue with my sample prep back here in our lab 
(550-551I).

Thanks,
Bree


On Wednesday, May 18, 2005, at 13:32 US/Pacific, Mary Tang wrote:

> Hi Bree --
>
> These should not be a problem.  However, there are a few concerns, 
> which I think we can pretty readily address.
>
> 1.  Many of these are solid.  We don't allow powders into the clean 
> room.  However, these can be mixed up in the wet benches in the 
> wafersaw room.  There is a metal bench for solvents and a polypro one 
> for acids/bases/water.  There is also a balance (although not a high 
> resolution one.)  Once these are mixed, they can be transferred to the 
> lab through the "gray area" behind the furnaces (where flammables are 
> normally stored.)  Ask one of us and we can show you.
>
> 2.  You'll need a barcode and a yellow hazardous tag for any bottles 
> you wish to store.  If you plan to get rid of them at the end of the 
> day, then a blue hazardous tag is all that is needed.
>
> 3.  You should probably use the headway instead of the laurell.  
> Mahnaz can correct me on this.  But it is a lot easier to handle solid 
> waste using the headway (you just line the bowl with foil and then 
> remove and place it in a hazardous waste bag when you are done.  
> Getting rid of waste is hopefully not a problem, since you will be 
> spinning on relatively small amounts.  This will probably all be 
> absorbed by your solid waste.
>
> 4.  Do you plan to do any heat treatment/activation following spin 
> coat?  Will there still be a lot of solvent on your wafers without 
> heating?
>
> Fellow SpecMat'ers:  any other questions or comments to add?
>
> Mary
>
> Bree Sharratt wrote:
>
>> This is the* 6th of 6* (yay!) new materials requests. The first 3 and 
>> last 2 materials are all various types of adhesion promoters and the 
>> 4th is a catalyst. Here is a list, in email order, of the new 
>> materials:
>>
>> 1. Gamma-Methacryloxypropyltrimethoxysilane
>> 2. Gamma-Glycidoxypropyltrimethoxysilane
>> 3. Gamma-Aminopropyltrimethoxysilane
>> 4. Propylamine
>> 5. n-Propyl Titanate
>> *6. n-Propyl Zirconate (this email)*
>>
>> Since these are all being used for the same research project, the 
>> description of the project and method will not change in subsequent 
>> emails. The n-propyl titanate and n-propyl zirconate are Tyzor 
>> products and the general brochure has been included for materials 5 
>> and 6. Please let me know if I need to further explain.
>>
>> Thanks,
>> Bree*
>>
>> Contact Information:*
>> Bree Sharratt
>> coral login: bree
>> office: 550-555C
>> office phone: 650 725 2634
>> mobile phone: 650 283 4835
>> home phone: 408 252 5545
>> email: sharratt at stanford.edu
>> PI: Prof. Reinhold H. Dauskardt (Materials Science & Engineering)
>>
>> *Chemical:*
>> MSDS attached at the bottom of this email.
>>
>> Chemical name: n-propyl zirconate
>> Product name: "Tyzor" NPZ
>> SYNONYM: Zirconium(IV) propoxide, 70% in 1-propanol
>> SYNONYM: "Tyzor" NPZ
>> SYNONYM: Zirconium(IV) propoxide in flammable solvent
>> SYNONYM: Zirconium(IV) propoxide solution
>> SYNONYM: Zircon-n-propylate
>> SYNONYM: Zirconium-Propylate
>> SYNONYM: Tetrapropoxy zirconium
>> SYNONYM: Zirconium tetrapropoxide
>>
>>
>> Components:
>> zirconium tetrapropanolate CAS# 23519-77-9 70%
>> n-propyl alcohol CAS# 71-23-8 30%
>>
>> Stanford Chemical Storage Group: L: Non-Reactive Flammables and 
>> Combustibles, including solvents
>> Main Hazard Class: flammable
>> Additional Hazards: flammable, skin irritant, lung irritant, eye 
>> irritant
>>
>> *Secondary Chemicals Used with this Chemical:
>> *n-propanol
>>
>> *Supplier Information:
>> *DuPont
>> 1007 Market Street
>> Wilmington, DE 19898
>>
>> contact:
>> product info: 800 441 7515
>> CHEMTREC: 800 424 9300
>> medical emergency: 800 441 3637
>> www.dupont.com/tyzor/
>>
>> *Reason for Request: Please note that this description is repeated in 
>> subsequent requests!*
>> My experimental work involves exploring the effects of environmental 
>> factors (temperature, relative humidity) and loading conditions (load 
>> type, mean stress, frequency) on debonding of SiNx/Epoxy/SiNx 
>> sandwich specimens. After observing some interesting behavior, I am 
>> investigating the effect that interface chemistry has on debonding. 
>> To accomplish this I will be spin-coating wafer pieces, which will be 
>> sectioned from 8 inch Si/SiO2/SiNx wafers (provided by LSI Logic, 
>> Inc) and etched in 50:1 HF, with 5 different adhesion promoting 
>> films. These adhesion promoters were specially selected to mimic 
>> certain functional groups and curing processes observed in other 
>> material systems. The following is a list of adhesion promoters that 
>> will be used in this study (note that the first three are similar to 
>> AP3000 and AP8000 already certified for use at SNF):
>>
>> Gamma-Methacryloxypropyltrimethoxysilane
>> Gamma-Glycidoxypropyltrimethoxysilane
>> Gamma-Aminopropyltrimethoxysilane
>> n-Propyl Titanate
>> n-Propyl Zirconate
>>
>> The first three adhesion promoters are silanes. Silane solutions will 
>> be stored and prepared in another Stanford lab (Peterson Bldg 550, Rm 
>> 551I) as follows: 1 part adhesion promoter will be dissolved in 100 
>> parts deionized water, which will be diluted with 900 parts methanol 
>> to produce a 0.1 wt% solution. A few drops of propylamine will be 
>> added as a catalyst for the hydrolysis reaction (except for 
>> gamma-aminopropyltrimethoxysilane, which self-catalyzes). This method 
>> was used by Maura Jenkins (Stanford PhD 2002) and Jeff Snodgrass 
>> (Stanford PhD 2001) in preparing wafers with similar adhesion 
>> promoter films (AP3000 and AP8000) and is documented in "Important 
>> factors for silane adhesion promoter efficacy: surface coverage, 
>> functionality and chain length," also attached.
>>
>> The zirconate and titanate adhesion promoter solutions will be 
>> prepared to produce a 0.1 wt% solution using n-propanol. A few drops 
>> of water may be added to encourage hydrolysis, which will be 
>> determined iteratively based on the results of the spin-coated film.
>>
>> *Process Flow:*
>> For wafer pieces (Si/thermal SiO2/PECVD SiNx):
>> 1. wbsolvent - mix 1 part n-propyl zirconate:700 parts n-propanol - 
>> bottle, cap and bag
>> 2. wbgeneral - clean wafer pieces in 50:1 HF, water rinse and blow 
>> dry with N2, box
>> 3. transport adhesion promoter solution, in cart, to laurel
>> 4. laurel - spin-coat onto wafer pieces
>> For glass slides (UV ozone cleaned and boxed in 550-553B):
>> 1. sts - deposit 200 nm SiNx
>> 2. wbsolvent - mix 1 part n-propyl titanate:700 parts n-propanol - 
>> bottle, cap and bag
>> 3. transport adhesion promoter solution, in cart, to laure
>> 4. laurel - spin-coat onto wafer pieces
>>
>> *Amount and Form:*
>> n-propyl zirconate - 250 mL bottle, liquid form
>> to be added to adhesion promoter solutions
>>
>> *Storage:*
>> Storage group L: Non-Reactive Flammables and Combustibles, including 
>> solvents
>> Incompatible with: water and aqueous solutions (will hydrolyze 
>> rapidly)
>>
>> *Disposal:*
>> Liquid and solid (gloves, wipes, etc) waste will be collected 
>> locally, properly labeled and disposed of according procedures that 
>> will be determined with the safety committee.
>>
>> *Attachments:
>> *1. MSDS for n-propyl zirconate (NPZ)
>> 2. Tyzor NPZ product information sheet
>> 3. Tyzor general brochure
>>
>>
>>
>
>
> -- 
> Mary X. Tang, Ph.D.
> Stanford Nanofabrication Facility
> CIS Room 136, Mail Code 4070
> Stanford, CA  94305
> (650)723-9980
> mtang at stanford.edu
> http://snf.stanford.edu
>
>