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64 English Edition No.49 December 2017 Topics Takumi MORIYAMA Nataliya NABATOVA-GABAIN Spectroscopic Ellipsometry Application in Life Science Introduction Spectroscopic ellipsometry (SE) is a non-destructive optical technique based on the measurement of polarization state change, using linearly polarized white light beam reflected from the sample surface. The set up of SE is shown in Figure 1 . Information about sample properties and structure, like layer thickness (d) and optical constants (refractive index (n) and extinction coeffi- cient (k)) values is obtained from the analysis of ellipsometric angles (Ψ&Δ) using modeling approach. [1] SE is widely used in academy and industry in the following application fields: semiconductors, displays, solar cells, chemistry and metallurgy. In the semi- conductor industry, especially, SE is used for about 30 years. In addition to measurement of layer thickness and optical constants, SE can also determine materials band gap, composition and electrical properties (resistivity, carrier density and mobility). SE measurement could be performed on variety of dif- ferent solid substrates, like semiconductors, glasses, metals and plastics films. SE measurement could be also performed in the liquid ambient. In recent years, SE application is extended to the life science. In this article, we intro- duce two examples from this field. Application in Life Science Biocompatibility of DLC films [2] This work was done in collaboration with Tokyo Denki University. The pur- pose of this study was to find the correlation between optical properties of diamond-like carbon (DLC) films and their biocompatibility, using spectro- scopic ellipsometry. DLC films structure could vary from dia- mond-like to graphite-like, depending on the ratio of diamond bonds (sp 3 ) to graphitic bonds (sp 2 ). DLC films are known for their excellent mechanical, tribological and chemical stability properties. Recently, DLC films biocompatibility opened new fields for applications in biology and medi- cine, as protective coating which modify surface of implants like artificial blood ves- sels or heart valves, for example. However, the biocompatibility of DLC films is strongly affected by their structural proper- ties, which are changing due to film deposi- tion methods and conditions. Depending on Establishes a linear polarization Excitation head Xenon Lamp Halogen lamp Automatic goniometer Sample stage Measures output polarization state Detection head Scanning monochromator PMT/CCD Detector Analyzer Sample Polarizer Light Figure 1 Setup of spectroscopic ellipsometer (UVISEL)
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Page 1: T Topics Spectroscopic Ellipsometry Application in Life ...

64 English Edition No.49 December 2017

Topics

Spectroscopic Ellipsometry Application in Life ScienceTopics

Takumi MORIYAMA

Nataliya NABATOVA-GABAIN

Spectroscopic Ellipsometry Application in Life Science

Introduction

Spectroscopic ellipsometry (SE) is a non-destructive optical technique based on the measurement of polarization state change, using linearly polarized white light beam refl ected from the sample surface. The set up of SE is shown in Figure 1. Information about sample properties and structure, like layer thickness (d) and optical constants (refractive index (n) and extinction coeffi -cient (k)) values is obtained from the analysis of ellipsometric angles (Ψ&Δ) using modeling approach.[1]

SE is widely used in academy and industry in the following application fi elds: semiconductors, displays, solar cells, chemistry and metallurgy. In the semi-conductor industry, especially, SE is used for about 30 years. In addition to measurement of layer thickness and optical constants, SE can also determine materials band gap, composition and electrical properties (resistivity, carrier density and mobility). SE measurement could be performed on variety of dif-ferent solid substrates, like semiconductors, glasses, metals and plastics fi lms. SE measurement could be also performed in the liquid ambient. In recent years, SE application is extended to the life science. In this article, we intro-duce two examples from this fi eld.

Application in Life Science

Biocompatibility of DLC films[2]

This work was done in collaboration with Tokyo Denki University. The pur-pose of this study was to fi nd the correlation between optical properties of diamond-like carbon (DLC) fi lms and their biocompatibility, using spectro-scopic ellipsometry.

DLC fi lms structure could vary from dia-mond-like to graphite-like, depending on the ratio of diamond bonds (sp3) to graphitic bonds (sp2). DLC fi lms are known for their excellent mechanical, tribological and chemical stability properties. Recently, DLC fi lms biocompatibility opened new fi elds for applications in biology and medi-cine, as protective coating which modify surface of implants like artifi cial blood ves-sels or heart valves, for example. However, the biocompatibility of DLC fi lms is strongly affected by their structural proper-ties, which are changing due to fi lm deposi-tion methods and conditions. Depending on

Establishes a linearpolarization

Excitation head

Xenon LampHalogen lampAutomatic

goniometer

Sample stage

Measures output polarization state

Detection head

Scanning monochromator PMT/CCD

Detector Analyzer Sample Polarizer Light

Figure 1 Setup of spectroscopic ellipsometer (UVISEL)

Page 2: T Topics Spectroscopic Ellipsometry Application in Life ...

Technical Reports

65English Edition No.49 December 2017

Topics the method of preparation, DLC could be hydrogen free (a-C) or hydrogenated (a-C:H). As a result, it is important to evalu-ate correctly the property of DLC films.

In this work, various DLC films were deposited by chemical vapor deposition (CVD) methods on polyvinyl chloride (PVC), dimethyl polysiloxane (PDMS) and polystyerene (PS) dishes.[3] The cells were grown on these dishes using mouse-derived fibroblasts. The cell proliferation rate was evaluated by absorbance measurement. The DLC films were measured by SE, to determine refractive index. In Figure 2, cell prolifera-tion rate is shown as function of refractive index.

In the case of base material, dish without DLC coating, the cell proliferation rate is defined as 1. It was found that the cell proliferation rate increases for the lower refractive index. In this work, films with the high hydrogen concentration have lower refractive index. So it is considered that the high hydrogen content of DLC films accelerates the cell proliferation on their surfaces. This result shows that SE can be used to evaluate the biocompatibility of DLC films.

Demineralization and remineralization process of tooth surface[4]

This work was done in collaboration with Tokyo Medical and Dental University. The purpose was to demonstrate demineralization and remineral-ization process of tooth surface due to exposure to acid and saliva respectively. SE used to measure the tooth effective surface roughness, using model described in Figure 3, and calculate the difference before and after exposure to saliva. Toothbrushing was introduced to demonstrate weakness of the demineralized tooth surface after exposure to acid.

The experiment procedure of this study was as following. Firstly, teeth were exposed to acid to introduce the demineralization on the tooth surface. SE used to measure the initial effective roughness. Secondly, each tooth was dipped into saliva for different periods of time to follow the remineralization process. Thirdly, after brushing each tooth, thickness of teeth effective surface roughness was measured by SE after dip into saliva. The difference of effec-tive roughness was calculated.

As shown in Figure 3, with increasing dip time in saliva, the difference of

1.5

4.0

3.5

3.0

2.5

2.0

1.5

1.0

0.5

0.02.52

Refractive index

Cel

l pro

lifer

atio

n ra

te

Figure 2 Correlation between refractive index and cell proliferation rate[3]

(Correlation coefficient “r” = 0.71, Significant difference “P” = 0.0004)

(b)

Dip into saliva time [min.]

Diff

eren

ce o

f effe

ctiv

e ro

ughn

ess

[nm

]

(a)

Effective roughness [nm] = (L1*0.1) + (L2*0.3)

Tooth

Tooth (90%) + Void (10%)

Tooth (70%) + Void (30%) L2

L1

Figure 3 (a) Optical model of tooth and (b) difference of effective roughness after brushing as function of dip into saliva time..

Page 3: T Topics Spectroscopic Ellipsometry Application in Life ...

66 English Edition No.49 December 2017

Topics

Spectroscopic Ellipsometry Application in Life Science

References

[ 1 ] S. Hirakawa, et al., HORIBA Technical Reports English edition, 19, 5 (2003)[ 2 ] Japan patent publication number 2014-57578[ 3 ] Y. Murayama, et al., Abstract of 2016 Hong Kong International Conference on Engineering and

Applied Sciences, HKICEAS-4905[ 4 ] Japan patent publication number 2016-128780

effective surface roughness was decreasing. This result demonstrates the rem-ineralization effect of saliva on demineralized tooth surface. From this result, it could be suggested that toothbrushing after meals should be done not imme-diately, but after some time, to allow saliva repair the tooth surface. The above result shows that SE can be used to evaluate the demineralization and the remineralization process of tooth surface.

Summary

SE is relatively inexpensive and quick method for characterization and optimi-zation of DLC fi lm properties to match relevant biomedical application. SE could be used to study the demineralization and the remineralization process of tooth surface. It also could be used for other medical application like devel-opment of artifi cial saliva. We hope to increase life science application of SE in the near future.

Acknowledgement

We would like to thank Prof. Kenji Hirakuri from Tokyo Denki University, Dr. Alireza Sadr, Dr. Shoji Nakashima, Dr. Yuichi Kitasako and Prof. Junji Tagami from Tokyo Medical and Dental University for fruitful discussions and permission to introduce the results in this article.

Takumi MORIYAMA, Ph.D.Analytical Technology CenterHORIBA TECHNO SERVICE Co., Ltd.

Nataliya NABATOVA-GABAINManagerGlobal Strategy DivisionHORIBA TECHNO SERVICE Co., Ltd.


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