WO2007015115A1 - Determination en temps reel, in situ, de l'epaisseur, des proprietes optiques et de la qualite de revetements transparents - Google Patents

Determination en temps reel, in situ, de l'epaisseur, des proprietes optiques et de la qualite de revetements transparents Download PDF

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Publication number
WO2007015115A1
WO2007015115A1 PCT/GR2006/000035 GR2006000035W WO2007015115A1 WO 2007015115 A1 WO2007015115 A1 WO 2007015115A1 GR 2006000035 W GR2006000035 W GR 2006000035W WO 2007015115 A1 WO2007015115 A1 WO 2007015115A1
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properties
fact
optical
real
thickness
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PCT/GR2006/000035
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English (en)
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Stergios Logothetidis
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Stergios Logothetidis
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Priority to US11/920,465 priority Critical patent/US7777882B2/en
Priority to EP06765394.9A priority patent/EP1910804B1/fr
Publication of WO2007015115A1 publication Critical patent/WO2007015115A1/fr

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Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
    • G01B11/00—Measuring arrangements characterised by the use of optical techniques
    • G01B11/02—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness
    • G01B11/06—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material
    • G01B11/0616—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating
    • G01B11/0683—Measuring arrangements characterised by the use of optical techniques for measuring length, width or thickness for measuring thickness ; e.g. of sheet material of coating measurement during deposition or removal of the layer
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21—Polarisation-affecting properties
    • G01N21/211—Ellipsometry
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/21—Polarisation-affecting properties
    • G01N21/211—Ellipsometry
    • G01N2021/213—Spectrometric ellipsometry

Definitions

  • This method can be used in-line for the monitoring and/or control of the production processes (in air and in vacuum), that concern substrates on which the thin films will be grown, and of the growth processes of transparent oxides, nitrides and other inorganic and organic films with final result the production of integrated
  • Spectroscopic Ellipsometry is a non destructive optical technique that is based on the measurement of the change of the light polarization state and provides information for the optical, and not only, materials properties. Spectroscopic Ellipsometry can be used for the in-situ and real-time monitoring during growth of inorganic and organics thin films, for the
  • Optical quantities such as the energy in which appears the maximum electronic absorption in a composite material, known as mean Gap or Perm Gap (E 0 ), and the energy where the edge of electronic absorption appears, known as the fundamental optical energy gap (E g ), are the ones that are directly related with their composition.
  • E 0 mean Gap or Perm Gap
  • E g fundamental optical energy gap
  • an appropriate, smart and reliable control process must: a) control the technical requirements for coatings (e.g. good adhesion of the substrate) in new applications, b) provide material and energy reduction and c) keep low the cost of combined processes.
  • This new methodology was applied in deposition processes of thin and transparent oxides on semiconducting but also polymeric substrates, as well as in pretreatment processes of polymeric substrates for the activation of their surfaces, on which later are grown transparent thin films such as Silicon Oxide (SiO x ), Titanium Oxide (TiO x ), Silicon Nitride (SiN x ) for various technological applications.
  • SiO x Silicon Oxide
  • TiO x Titanium Oxide
  • SiN x Silicon Nitride
  • the thickness and deposition rate of transparent films are determined with high accuracy.
  • the use of the geometrical model consisted by three phases (air/thin film/polymeric substrate) in the analysis of the SE spectra deducted during oxide deposition, provides the ability to determine the thickness d of the transparent inorganic (oxide, nitride, etc) and organic film. With this analysis, the stability and effectiveness of the deposition processes can be controlled and monitored.
  • the deposition processes of the transparent oxides films are monitored in real-time.
  • the E 0 is related to the stoichiometry x of the film
  • the barrier properties in gases and vapors of the system thin film/polymeric substrate are determined. This determination is the result of the correlation between the optical and other properties of the system that were measured in real-time with the above mentioned methodology (e.g.
  • the methodology that has been developed can be used in-line for the monitoring and control of the various vacuum processes of the substrates on which the thin films will be grown, and for the growth process of transparent inorganic (oxides and nitrides) or and organic films, to finally result in the production of complete systems, with desirable properties.
  • This is especially important for the control of production & manufacturing processes in real-time and for the minimization of the time needed for production control, of the losses and of the production cost.
  • FIGURE 1 Schematic representation of the in-situ Fourier Transform IR Spectroscopic Ellipsometer (FTIRSE) adjusted in a Ultra High Vacuum Chamber.
  • FTIRSE Fourier Transform IR Spectroscopic Ellipsometer
  • FIGURE 2 Spectra of the imaginary part ⁇ 2 (E)> of the dielectric function during the surface treatment of the polymeric substrate Poly(Ethylene Terephthalate) (PET) with Nitrogen (N 2 ) ion bombardment by Pulsed DC Plasma Etching.
  • FIGURE 3 Schematic representation of the ex-situ of Spectroscopic Ellipsometry unit of the near infrared (Near IR)-Visible-Far Ultraviolet (Visible - FUV) spectral region.
  • FIGURE 4 The ⁇ 2 (E)> spectra in real-time during SiO 2 thin film growth on polymeric substrate PET, with e-beam evaporation technique and with the evaporation SiO 2 material.
  • the triangles correspond to the measured imaginary part ⁇ 2 (E)> of PET before the SiO 2 deposition, while the circles correspond to the ⁇ 2 (E)> of SiO 2 .
  • FIGURE 5 The ⁇ 2 (E)> spectra in real-time during SiO thin film growth on polymeric substrate PET 5 with e-beam evaporation technique and with the evaporation of SiO material.
  • the triangles correspond to the measured imaginary part ⁇ 2 (E)> of PET before the SiO deposition, while the circles correspond to the ⁇ 2 (E)> of SiO.
  • FIGURE 6 The ⁇ 2 (E)> spectra in real-time during SiO x thin film growth on polymeric substrate PET, with e-beam evaporation technique and with the evaporation mixed SiO and SiO 2 material.
  • the triangles correspond to the measured imaginary part ⁇ 2 (E)> of PET before the SiO x deposition, while the circles correspond to the ⁇ 2 (E)> of SiO x .
  • FIGURE 7 Time dependence of the thickness, the Penn gap E 0 and the energy gap E g of the SiO x thin film grown on the PET polymeric substrate. The results were obtained with the real-time analysis of the SE spectra measured by the FMWE unit.
  • FIGURE 8 Time dependence of the thickness of the SiO x thin film grown on the PET polymeric substrate by electron beam evaporation of SiO. The results were obtained with, the real-time analysis of the SE spectra measured by the FMWE unit.
  • FIGURE 11 Evolution of the thickness of SiO 2 , SiO and SiO x films during the first 50 s of their growth process.
  • FIGURE 12 Evolution of E 0 Of SiO 2 , SiO and SiO x films during the first 50 s of their growth process.
  • FIGURE 13 Evolution of E g Of SiO 2 , SiO and SiO x films during the first 50 s of their growth process.
  • PET Poly(Ethylene Terephthalate)
  • PVD Physical or Chemical Vapor Deposition techniques
  • This methodology can be generally applied in the case of monolayered and multilayered, transparent and non- transparent thin films, that can be comprised only of (or combination of) thin films of Silicon Oxide (SiO x ), Titanium Oxide (TiO x ), Silicon Nitride (SiN x ), Titanium Nitride (TiN x ), Zinc Oxide (ZnO x ), Boron Nitride (BN x ), Carbon Nitride (CN x ), Aluminium Oxide ⁇ (AlO x ) for all the stoichiometry values x that are developed with the various Physical and Chemical Vapor Deposition growth techniques, such as magnetron sputtering (dc, rf or/and reactive), e-beam evaporation, ion beam sputtering, ion beam assisted deposition, CVD, Plasma Enhanced CVD, laser, ablation, laser deposition.
  • SiO x Silicon Oxide
  • TiO x Titanium Oxide
  • PET Poly(Ethylene Terephthalate)
  • PEN Poly(Ethylene Naphthalate)
  • PES Polyethylene Sulfate
  • PC PolyCarbonate
  • PA Polyamide
  • PP Polypropylene
  • PVC Polyvinyl Chloride
  • PTFE PolyTetraFluoroEthylene
  • the realization of measurements in such short time is in accordance with the one needed for the real-time control of thin films that are grown with deposition rate of ⁇ 5 A/s, such as the SiO x thin films growth on a PET polymeric substrate.
  • Spectroscopic Ellipsometry- SE measurements ( Figure 1) in the spectral region of Visible- Far Ultraviolet (Vis-FUV) were realised with a Fast MultiWavelength Ellipsometer (FMWE) unit that was developed in collaboration with Horiba/Jobin-Yvon, while the SE measurements in the spectra area of Infrared (IR) were realised with the Fourier Transform IR Spectroscopic Ellipsometer (FTIRSE) unit. Both units are adjusted on a ultra high vacuum chamber where the angle of incidence is 70°. Other angles, lower or higher, from 70° can also be used.
  • FMWE Fast MultiWavelength Ellipsometer
  • FTIRSE Fourier Transform IR Spectroscopic Ellipsometer
  • the chamber is equipped with various Physical Vapor Deposition techniques (PVD) while for the thin films growth on polymeric substrates is used the e-beam evaporation technique.
  • PVD Physical Vapor Deposition techniques
  • the substrate holder on which the substrate is adjusted is positioned horizontally on stable position and it has the capability to rotate around a vertical axis.
  • the SE measurements are performed in the spectra are of the Visble- Far Ultraviolet (Vis-FUV) from 1.5 - 6.5 eV (190 - 830 nm), and in the spectra area of IR, 0.1 - 0.49 eV (900 - 4000 cm "1 ).
  • the realization of the measurements in the spectra area of Vis-FUV are applied for the study of the material's optical properties (bulk materials and thin films), that are related to the electronic transmissions, their electronic structure and their thickness.
  • the real-time measurement is performed with the simultaneous acquisition of 32 different wavelengths (32 simultaneously measured data points) that cover the energy range of 1.5 - 6.5 eV.
  • the upper energy limit of SE spectra acquisition with the use of FMWE is 6.5 eV (190 nm), and with which can be performed the control of the polymeric membranes' and grown thin films optical properties.
  • the deposition rates of the oxide films, that have been referred are significantly lower in comparison to the ones in industrial scale, so the evaporation process on stable or moving substrate is more controllable and repeatable and the grown thin films show higher density values than the ones that are produced on moving substrates with the form of rolls (roll-to- roll) or in in-line roll-to-roll production on industrial scale,
  • these processes can be applied in an in-line constant production and industrial scale.
  • the parameterization and analysis of the measured pseudo-dielectric function ⁇ (E)> ⁇ i(E)>+i ⁇ 2 (E)> has been performed with the use of a geometrical model consisted by three phases (air/thin film/polymeric substrate) in which the determination of the optical properties of each phase has been realized with the modified Tauc-Lorentz (TL) model.[l] In the case where the surface modification of the polymeric substrate is measured, the thin film represents the modified layer. In the TL model the imaginary part ⁇ 2 (E) of the dielectric function is determined by multiplying the Tauc density of states with the ⁇ 2 that results from the Lorentz oscillator model.
  • the TL model provides the capability of determining the fundamental optical gap Eg of the interband transitions, the energy EO, the broadening C and the strength A of each oscillator.
  • the EO of this model is correlated to the known Penn gap, the energy position where the strong electronic absorption of the material, mainly amorphous, takes place.
  • the imaginary part E 2 (E) of the TL oscillator, for both amorphous and crystalline materials, is given by the following relations:
  • the basic information deduced by SE measurements/analyses concerns the film thickness, and the optical parameters and constants, which are strongly related to films' stoichiometry and quality. More specifically, it can be calculated:
  • the ⁇ ⁇ that measures the material strength and accounts the contribution of all electronic transitions, even those not taken into account in the modeling analysis, because they occur at high energies well above the experimental measured energy range, otherwise it is equal to unity.
  • the most important that are determined by the spectra analysis are the Penn gap E 0 and the refractive index n.
  • the EO is directly related to films' stoichiometry
  • Figure 2 shows the measurement of the optical properties by the use of FTIRSE in real-time, during the surface treatment of Poly(Ethylene Terephthalate) (PET) polymeric substrate with Nitrogen (N 2 ) atoms using Pulsed DC Plasma Etching.
  • the partial pressure of the chamber was ⁇ 30 mTorr and the gas flow remained constant at 40 seem, whereas the voltage applied on the substrate holder through the high voltage pulse modulator (Advanced Sparc-le V) was 700V with frequency of 100 Hz.
  • the surface treatment process has duration of 20 min.
  • the imaginary part ⁇ 2 (E)> is presented.
  • the thickness d of the SiO x thin film deposited onto PET can be determined.
  • Figure 7 shows an example of the determination of thickness d as a function of the deposition time during the sample rotation, form which we can evaluate and control in-line the deposition process stability and effectiveness.
  • the change of the deposition conditions affects the deposition rate of the SiO x thin films, as it can be seen at the points a, b, c and d in Figures 8 and 9.
  • the information that is obtained from the analysis of the measured SE spectra, in-situ and real-time is very important for industrial scale.
  • the Penn gap Eo exhibits a monotonic increase and an almost linear correlation with the stoichiometry (e.g. SiO x ).
  • B 0 for SiO 2 depending on its amorphous or crystalline microstructure that is 10.5 and 12 eV, respectively.
  • This methodology provides accurate results, rendering suitable for the characterization and the control of the properties and the quality of thin transparent films, inorganic and organic materials that are developed in polymeric substrates or other transparent substrates.
  • Figure 11 shows the comparative results from the real-time analysis of SE spectra in the Vis - FUV spectral region, from three SiG x thin films that were deposited onto polymeric substrate (PET) by electron beam evaporation of three different materials SiO 2 , SiO, and SiO x (mixed SiO + SiO 2 ). From this figure we observe the dependence of thickness as a function of deposition time from which we conclude that in small thicknesses the nucleation and coalescence stages take place, which are followed by the homogenous growth stage. From this dependence we can determine the deposition rate of the each film (6.4, 3.7 and 2.8 A/s, for SiO 2 , SiO and SiO x , respectively).
  • Figures 12 and 13 show the evolution of the Eo and E g parameters with the deposition time, as determined with the above methodology.
  • the determination of the barrier properties for gases and water vapours of the SiO x /PET system is accomplished with the correlation the optical and other properties of system, that were measured in real-time with the above methodology (e.g. stoichiometry x), with the penetrability measurements for oxygen (OTR) and water vapours (WVTR).
  • OTR oxygen
  • WVTR water vapours

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Abstract

Cette invention concerne la détermination en temps réel, in situ, de l'épaisseur, des propriétés optiques et de la qualité de films minces inorganiques transparents (oxydes, nitrures) et de matériaux inorganiques pendant leur développement et pendant la modification de matériaux polymères transparents, ceci par éllipsométrie spectroscopique, avec des mesures dans la région spectrale des Vis- FUV comprise entre 1.5 et 6.5 eV, et des infrarouges (IR) entre 0.1 et- 0.49 eV (900-4000 cm-1). Cette technique peut être utilisée en ligne pour le contrôle et/ou la commande de processus à l'air libre ou et sous vide pour des substrats sur lesquels seront tirés des films minces et pour le développement d'oxydes et de nitrures transparents et de films inorganiques, le résultat final étant l'obtention de systèmes intégrés aux propriétés recherchées.
PCT/GR2006/000035 2005-08-01 2006-07-24 Determination en temps reel, in situ, de l'epaisseur, des proprietes optiques et de la qualite de revetements transparents WO2007015115A1 (fr)

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US11/920,465 US7777882B2 (en) 2005-08-01 2006-07-24 Method for the in-situ and real-time determination of the thickness, optical properties and quality of transparent coatings during their growth onto polymeric substrates and determination of the modification, activation and the modification depth of polymeric materials surfaces
EP06765394.9A EP1910804B1 (fr) 2005-08-01 2006-07-24 Determination en temps reel, in situ, de l'epaisseur, des proprietes optiques et de la qualite de revetements transparents

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Cited By (14)

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CN102507875A (zh) * 2011-11-09 2012-06-20 复旦大学 一种快速无损测量石墨烯薄膜厚度与能带结构的方法
CN103323403A (zh) * 2013-05-27 2013-09-25 浙江大学 一种低辐射镀膜玻璃的光学参数检测方法
US9371577B2 (en) 2013-12-31 2016-06-21 Halliburton Energy Services, Inc. Fabrication of integrated computational elements using substrate support shaped to match spatial profile of deposition plume
US9395721B2 (en) 2013-12-24 2016-07-19 Halliburton Energy Services, Inc. In-situ monitoring of fabrication of integrated computational elements
US9495505B2 (en) 2013-12-24 2016-11-15 Halliburton Energy Services, Inc. Adjusting fabrication of integrated computational elements
US9523786B2 (en) 2014-03-21 2016-12-20 Halliburton Energy Services, Inc. Monolithic band-limited integrated computational elements
US9708908B2 (en) 2014-06-13 2017-07-18 Halliburton Energy Services, Inc. Integrated computational element with multiple frequency selective surfaces
US9727052B2 (en) 2014-02-14 2017-08-08 Halliburton Energy Services, Inc. In-situ spectroscopy for monitoring fabrication of integrated computational elements
US10247662B2 (en) 2013-07-09 2019-04-02 Halliburton Energy Services, Inc. Integrated computational elements with frequency selective surface
US10496776B2 (en) 2013-12-24 2019-12-03 Halliburton Energy Services, Inc. Fabrication of critical layers of integrated computational elements
US10718881B2 (en) 2013-07-09 2020-07-21 Halliburton Energy Services, Inc. Integrated computational elements with laterally-distributed spectral filters
US10914863B2 (en) 2013-12-24 2021-02-09 Halliburton Energy Services, Inc. Real-time monitoring of fabrication of integrated computational elements
CN114018820A (zh) * 2021-09-14 2022-02-08 深圳市埃芯半导体科技有限公司 光学测量方法、装置、系统及存储介质
US11274365B2 (en) 2013-12-30 2022-03-15 Halliburton Energy Services, Inc. Determining temperature dependence of complex refractive indices of layer materials during fabrication of integrated computational elements

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Cited By (16)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102507875A (zh) * 2011-11-09 2012-06-20 复旦大学 一种快速无损测量石墨烯薄膜厚度与能带结构的方法
CN103323403A (zh) * 2013-05-27 2013-09-25 浙江大学 一种低辐射镀膜玻璃的光学参数检测方法
CN103323403B (zh) * 2013-05-27 2015-04-15 浙江大学 一种低辐射镀膜玻璃的光学参数检测方法
US10247662B2 (en) 2013-07-09 2019-04-02 Halliburton Energy Services, Inc. Integrated computational elements with frequency selective surface
US10718881B2 (en) 2013-07-09 2020-07-21 Halliburton Energy Services, Inc. Integrated computational elements with laterally-distributed spectral filters
US10914863B2 (en) 2013-12-24 2021-02-09 Halliburton Energy Services, Inc. Real-time monitoring of fabrication of integrated computational elements
US9495505B2 (en) 2013-12-24 2016-11-15 Halliburton Energy Services, Inc. Adjusting fabrication of integrated computational elements
US10496776B2 (en) 2013-12-24 2019-12-03 Halliburton Energy Services, Inc. Fabrication of critical layers of integrated computational elements
US9395721B2 (en) 2013-12-24 2016-07-19 Halliburton Energy Services, Inc. In-situ monitoring of fabrication of integrated computational elements
US11274365B2 (en) 2013-12-30 2022-03-15 Halliburton Energy Services, Inc. Determining temperature dependence of complex refractive indices of layer materials during fabrication of integrated computational elements
US9371577B2 (en) 2013-12-31 2016-06-21 Halliburton Energy Services, Inc. Fabrication of integrated computational elements using substrate support shaped to match spatial profile of deposition plume
US11066740B2 (en) 2013-12-31 2021-07-20 Halliburton Energy Services, Inc. Fabrication of integrated computational elements using cylindrical substrate support shaped to match a cross-section of a spatial profile of a deposition plume
US9727052B2 (en) 2014-02-14 2017-08-08 Halliburton Energy Services, Inc. In-situ spectroscopy for monitoring fabrication of integrated computational elements
US9523786B2 (en) 2014-03-21 2016-12-20 Halliburton Energy Services, Inc. Monolithic band-limited integrated computational elements
US9708908B2 (en) 2014-06-13 2017-07-18 Halliburton Energy Services, Inc. Integrated computational element with multiple frequency selective surfaces
CN114018820A (zh) * 2021-09-14 2022-02-08 深圳市埃芯半导体科技有限公司 光学测量方法、装置、系统及存储介质

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