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### Study Report

Title: Characterization of Test Substance Oxygen Functional Group Distribution



### Report Date: October 30, 2014



### File Reference:

Principal Investigator(s): {

}



### Tes ting Facility: {

}


### Spon sor: {



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TS -ZF02NT

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### Study Report

Characterization of Test Substance Oxygen Functional Group Distribution

Introduction: X-ray photoelectron spectroscopy is used in conjunction with chemical derivitization to examine the distribution of oxygen containing functional groups } present in the Sponsor’s Test Substance.



### 1) Purpose & Scope: This study provides characterization data on the distribution of oxides present in the Sponsor’s Test Substance in normal liquid suspensions (Test Solution). This summary is to be used to inform chemical identification processes {, }.


### 2) Adm inistrative Organization: This report was prepared by principal investigator, { based upon chemical deriviti zation and subsequent XPS analysis carried out by {

}

. 

### 3) Test Sub stance: The study was conducted on the TS -ZF02NT new chemical substance (Test Substance) wi thout confounding { typical of the final for mulation.



### 4) Pri nciple and Study Design: X-ray photoelectron spectroscopy is a surface sensitive technique (5-10nm) using the binding energies of core level electrons to determine elemental surface composition and oxidation state of a material. For {

} fitting becomes ambiguous and derivitization of specific oxide functional groups with F luorinated tags (which are more sensitive in the XPS) is needed for quantification. A sepa rate sample is needed for each oxide being assayed. Further details may be found in the attached report.


### 5) Sample Handling and Preparation: The new chemical substance was provided to { } and prepared under his direc tion after the pilot centrifugation process, but {

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TS -ZF02NT

3 was mounted to a blank 200mm wafer used for shipment purposes only. The prepared sample

wa s enclosed in a standard 200mm wafer case, and taped closed with FAB tape. Final packaging and transfer to the UPS carrier was by { } Shipping and Receiving. The sample was shipped intact, in a secure container to the Testing Facility.


### 6) Study Results: {

}


### Appendices:

1. { }Report Prepared by:

The goal of this project was to characterize the oxygen functional group distribution in films prepared
from Type B using chemical derivatization coupled to X

- ray photoelectron spectroscopy (XPS).



### XPS Overview.

X-ray photoelectron spectroscopy (XPS) is a surface analytical technique (top 5-10 nm) used for elemental analysis of samples under ultra-high vacuum conditions ( 10 -8

- 10 -9 Torr). Both identification and quantification of the atomic composition is achieved by incident X-rays of a specific photon energy causing core level electrons of a sample to eject at various kinetic energies. Since each element has a unique set of core electron binding energies, the specific kinetic energy at which a particular core level electron is ejected will allow for elemental identification while the number of detected electrons at this particular energy will enable the quantification of this element relative to other elements in a given sample.



### Initial Survey Scan.

XPS analysis typically begins with a scan across a wide range of energies to identify the elements present in a particular sample at concentrations greater than 1%. In a survey spectrum, the energy is reported as binding energy. For the sample analyzed, Type-B, the only elements
identified were , indicating that there were no contaminants containing other elements and the coating of completely covered the underlying substrate.

### Quantitative Analysis.

Chemical Derivatization

Chemical derivatization is a labeling technique used to tag specific functional groups on a surface. Three derivatizing reagents, all containing fluorine, can be used to tag The reactions are carried out in the vapor phase to minimize purification and work-up steps. The % fluorine (1s) for each derivatization reaction can be quantified using XPS andstoichiometrically used to determine the percentage of each oxygen functional group. The derivatization

reactions are outlined below:



### Analysis of Oxygen Functional Group Distribution

Type B samples were run in triplicate for each chemical derivatization reaction. The highest concentration of tagged oxygen functional group was observed for the

synthesis method or the preparation procedure. Regardless, all derivatization reactions were observed to have good precision, with a
standard deviation of ± 0.1%.