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

Mary Tang mtang at
Wed May 18 13:32:43 PDT 2005

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?


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
> 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
> *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
mtang at

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