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Surface Engineering Research for Bio-Medical & Medical Electronics Applications in 2010:  NanoBonding™ and VitreOX™
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Surface Engineering Research for Bio-Medical & Medical Electronics Applications in 2010: NanoBonding™ and VitreOX™

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This overview of N. Herbots's SiO2 group research on Surface Engineering for Bio-Medical and Medical Electronics in 2010 describes the background to our nest technologies in NanoBonding™ and …

This overview of N. Herbots's SiO2 group research on Surface Engineering for Bio-Medical and Medical Electronics in 2010 describes the background to our nest technologies in NanoBonding™ and VitreOX™.

PATENTS & TECHNOLOGY DISCLOSURES RELATED TO THIS RESEARCH:
[1] Methods for Wafer Bonding & for Nucleating Bonding Nanophases Using Wet and Steam Pressurization, N. Herbots, S.D. Whaley, R.Bennett-Kennett, R.J. Culbertson, A.M. Murphy, S.J. Farmer, US Patent filed 10/ 31/2011
[2] Molecular Film Containing Polymeric Mixture for Hydrophobic Implant Surfaces N. Herbots, A, M. Murphy, R. Kennett-Bennett, D.A. Sell S.D. Whaley, R.J. Culbertson, US Patent filed 11/3/ 2011
[3] ASU/AZTE Technology Disclosure M11-163P "H2O Nano-­‐Bonding “ Synthesis via compressive strain from sursaturated water vapor at low temperatures (T< 175°C) of a siloxane-­‐silica mixed nano-­‐bonding phase catalyzed by H2O, nano-scale smoothing and ordering of Si(100) & silica, and room temperature chemical reactivity arising from surface polarization through surface charge generation in SiO2. N. Herbots, S.D. Whaley, R. Bennett-Kennett, R.J. Culbertson, A.M. Murphy, S.J. Farmer, filed June 24th, 2011

[4] ASU/AZTE Technology Disclosure M11-164 P ProteinKnox" - A Temporary and Permanent Surface Bio-Compatible Adsorbate to Control in Conjunction with Hydroaffinity the Blood Proteins Adsorption, Build-up and/or Clot Formation on Surface of Medical Implant Devices and Grafts using LVPL's (Low Viscosity Polar Liquids)" , filed June 24th, 2011

[5] A Method for Wafer Bonding and for Nucleating Bonding Nanophases
N. Herbots, J. D. Bradley, M. Hart, D. A. Sell, S. D. Whaley, R.J Culbertson Provisional Patent Application SN 61/174,138 , ASU/AZTE (filed 3/30/2009).
 
Molecular films for controlling hydrophobic, hydrophilic, optical, condensation and geometricproperties of silicone implants surfaces, including intra-occular lenses used in cataract surgeries. N. Herbots, J. D. Bradley, M. Hart, D. A. Sell & S. D. Whaley
ASU/AZTE (filed 3/30/2009). Provisional patent application filed October 2, 2009
 
Methods for Wafer Bonding and for Nucleating Bonding Nanophases Using Wet and Steam Pressurization, N. Herbots, S.D. Whaley, Ross Bennett-Kennett, R.J. Culbertson, A.M. Murphy, S.J. Farmer, US Patent filed 10/31/11

CONFERENCE PRESENTATIONS
[1] Nanobonding between 2-nm β-crystobalite SiO 2 on OH(1x1)Si(100) & SiO x for Monolithic Electronics by Surface Smoothing via Wet Chemical and Spin Processing: TMAFM Study and Modelling of Interphases “ S.D. Whaley, N. Herbots, J.D. Bradley, R.J. Culbertson, M.A. Hart, D.A. Sell, Q.X. Bradley, R.L.Rhoades, S.N. Drews, R.B. Bennett-Kennett, 58th International American Vacuum Society Symp, Nashville, TN, Oct 31-Nov. 4th, 2011
[2] Controlling the Hydroaffinity of Silicone/Hydrophobic Acrylic Surfaces of Intraocular
Lenses using Visco-Elastic Colloids and Blood Proteins, N. Herbots, R.J. Culbertson, Q.X. Bradley, D.A


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  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • ASU - Physics - Emeritus College - NanoScience, Materials Physics &amp; Biophysics
  • Transcript

    • 1.
    • 2. FACULTY AND STUDENTS + Department of Physics, ASU Prof. Nicole Herbots * , emeritus Prof. R.J. Culbertson Dr. J. D. Bradley * , Visiting Scientist, Medtronic Corporation Shawn Whaley * & Qian Bradley * , graduate students David Sell* & Murdock Hart, undergraduate Res. Assist, COLLABORATORS Dr. Clive Sell * , MD, vitro-retineal surgeon Dr. Mark Kwong, Chem. Eng., MD, ophtamological surgeon John Mitchell *, Comp. Eng., MBA, CEO Clarizza Watson *, Chem. Eng., MBA, Marketing + Funded by Royalties from US patent 6,613,677 AZ ABOR Tech ASU Strategic Initiative Fund Emeritus College Grant , Bausch & Lomb Donation Associated Retina Consultance. LLC * SiO2 Associates, Founders & Members
    • 3. FACULTY AND STUDENTS + Department of Physics, ASU Prof. Nicole Herbots*, emeritus Prof. R.J. Culbertson Dr. J. D. Bradley*, Visiting Scientist, Medtronic Corp. Shawn Whaley* & Qian Bradley*, graduate students David Sell* &Murdock Hart, undergr. Res. Assist, Maggie Mitchell, Administrative Assistant
    • 4. COLLABORATORS Dr. Clive Sell * , MD, vitro-retineal surgeon Dr. Mark Kwong, Chem. Eng., MD, ophtamological surgeon John Mitchell *, Comp. Eng., MBA, CEO Clarizza Watson *, Chem. Eng., MBA, Marketing + Funded by Royalties from US patent 6,613,677 AZ ABOR Tech ASU Strategic Initiative Fund Emeritus College Grant , Bausch & Lomb Donation Associated Retina Consultance. LLC * SiO2 Associates, Founders & Members
    • 5. Expertise
      • CONTROL OF SI SURFACES AT THE ATOMIC SCALE
        • Creation of highly planar ordered surfaces
        • Control of surface electrical properties
        • Control of hydro-affinity of surfaces
        • Creation of hermetic seals by direct atomic bonding
    • 6. Motivation
      • BIOMEDICAL ENGINEERING
      • 1. Cure Medical Complications From Cataracts
      • stop condensation on hydrophobic lenses during surgery
      • How to inhibit condensation on a surface?
      • 2 . Create Implantable Medical Sensor e.g. an Artificial Pancreas
      • bond hermetically silica into an implantable glucose monitor
      • How to connect two silica surfaces as if they were one?
      • SCIENTIFIC
      • understanding surface condensation , hydroaffinity (attraction to water) …. And .... bonding at the nanoscale
      • How do water molecules interact with Si, SiO 2 , Silicone,
      • acrylics …. Polymers … any material ..
    • 7. Outline
      •   1. SCIENTIFIC MODELS & Discoveries
      • • 3-D String, RasMol, patents on Si(100) & SiO 2
      • • hydrophobic/hydrophilic surfaces of Si(100) & SiO 2
      • 2. EXPERIMENTAL PROCEDURES: Laboratories
      • clean-room, wet chemical laminar hoods
      • • synthesis, contact angle, bonding & condensation
      • on Si(100) crystal, SiO 2 , silicone, acrylic lenses, etc…
      • topography by Atomic Force Microscopy (AFM)
      • composition by Ion Beam Analysis (RBS, PIXE)
      • 3. RESULTS: 4 ASU Patents, two of which filed on 4/09 and 11/09
      • • “ Wafer bonding using a nanophase connecting both surfaces”
      • • “ Inhibition of condensation on surfaces ..” (Inter Occular Lenses)
    • 8. Nanoscience, materials physics, biophysics, artificial eye-lens & pancreas?
      • Artificial Eyelens Bio-Medical Challenge :
      • Modify the surface of a silicone lenticular implant so it
      • does NOT “fog” during surgery
      • Artificial Pancreas Bio-Medical Challenge
      • BOND a blood chemistry monitor (typically on quartz) directly to a single implantable device mounted on silicon wafers.
      • PHYSICS: Greatest Feat of 20 th Cent. “Contemporary Physics” Unification of Physics & Chemistry [Slater, Feyman] Greatest Feat of the 21 st Century “ New Physics ” : Unification of Physics with Biology?
    • 9. SCIENTIFIC MODELS: Understanding surface condensation , hydroaffinity, bonding at the nanoscale … How do water molecules interact with surfaces?
      • hydrophilic
      • hydrophobic
      Water molecules are electrical dipoles
    • 10. How do water molecules interact with each other or with surfaces?
      • hydrophilic
      • hydrophobic
      Water molecules interact with each other as electrical dipoles Water dipoles interact with FREE charges, defects, ions
    • 11. Medical MOTIVATION #1 How important is this problem? ] Vision at age 40 1 in 5 will develop cataracts 20M Americans have cataracts Cataracts are the leading cause of blindness in the world World Health Organization Everyone will develop cataracts One Cure – Cataract Surgery After Cataract Surgery Most Crystalens Patients Studied 20/40 or Better Bausch & Lomb Early Life Vision
      • Vision at age 65+
      • 50% cataract rate
        • National Health Institute
    • 12. Medical MOTIVATION #1 How important is cataract surgery? Most common surgery in the world 15 million cataract surgeries performed each year
    • 13. Motivation – access for all by removing problem
      • STOP condensation on hydrophobic IOL
      • during secondary
      • surgery, after cataract surgery
      • LET’s SOLVE THIS PROBLEM!
    • 14. SCIENTIFIC MOTIVATION understanding surface condensation , hydroaffinity …. And .... bonding at the nanoscale What is “nanoscale “?
      • Interspacing between atoms in a silicon crystal
      • or Si(100) surface = 2.5 nm
      • hermetically bond a blood chemistry sensor to a processor =
      • “ Nanobonding” with with an interphase
      “ Dangling” bonds Quartz Si (100) BEFORE AFTER Quartz Si (100)
    • 15. x y SCIENTIFIC MOTIVATION understanding surface condensation , hydroaffinity (attraction to water) …. And .... bonding at the nanoscale What is “nanoscale “,  how do water molecules interact ? SiO 2
    • 16. Ordered Oxide Patent, licensed to Intel
        • Foundational Patent covers
        • Herbots-Atluri clean
        • Ordered nanophases such as
        • ORDERED Si(100) hydroxyl terminated surface,
        • results in hydrophobic behavior
      Passivated Si(100) Surface OH OH OH OH
    • 17. 3. EXPERIMENTAL PROCEDURES: Laboratory : No sodium, CLASS 100 clean-room, hoods • synthesis, contact angle, bonding & condensation on Si(100) crystal, SiO 2 , silicone & acrylic lenses, - Atomic Force Microscopy (AFM) - surface composition by ion scattering (RBS, PIXE)
    • 18. • Chemical Fume and Laminar Flow Hoods OUTSIDE THE CLEAN ROOM FOR • experiments on silicone & acrylic IOL’s Use SALINE and Deionized (DI) Water (2 MegOhms, 18 MegOhms)
    • 19. Hydrophobic Acrylic IOL’s T = 38 °C All 4 IOL’s FOG Within 5 s
    • 20. How do water molecules interact with each other or with surfaces?
      • Model System ,
      • clean-room
      • • contact angle
      • Silicon surface Si(100)
        • Hydrophilic Silicon
        • Hydrophilic Silicon
      • Demonstration of passivated, terminated, ordered Si(100) regions
      • Next to a defect rich Si(100) region
      • Using metered water drops for contact angle measurements to qualify (1) hydrophobic and (2) hydrophilic behaviors
    • 21. EXPERIMENT: MEASUREMENT OF CONTACT ANGLES Direct Observation of silicone & acrylic lenses Silicone Lens Acrylic Lens
    • 22. EXPERIMENT: silicone & acrylic lenses’ surface topography by Atomic Force Microscopy (AFM)
        • Silicone surface is very smooth (Optically Superior)
        • Acrylic surface is rougher
    • 23. Immediate FOGGING Observed on BOTH Silicone & Hydrophobic Acrylic IOL’s NO Fogging After VitreOx on BOTH Silicone & Hydrophobic Acrylic IOL’s T = 38 °C Hydrophobic Acrylic IOL’s
    • 24. Hydrophobic Acrylic IOL’s T = 38 °C After VitreOx TM Identical treatment for two different materials!
    • 25. 4. RESULTS: Two ASU Patents “Inhibition of condensation on surfaces ..” (Inter Occular Lenses (IOL’s, etc..)
      • Dr. Clive Sell, MD smiles as he applies our bio-compatible treatment, “VITREOX” to render an IOL hydrophilic.
      • He has used the technique successfully
    • 26. What might an artificial pancreas look like? create an artificial pancreas = integrate (1) blood glucose sensor + (2) monitoring electronics hermetically into a single implantable device How to connect two silica surfaces as if they were one?
    • 27. The goal is to avoid painful “finger pricks” and CONTINUOUSLY monitor blood chemistry
      • http://www.medtronic-diabetes.com.au/images/launch/diagram_02.jpg
      create an artificial pancreas = integrate (1) blood glucose sensor + (2) monitoring electronics hermetically into a single implant device How to connect two silica surfaces as if they were one?
    • 28. The implanted monitor sends radio-waves to the insulin pump processor to activate the alarm (“ eat ”) or deliver insulin (“ fast ”)
    • 29. Practically, it boils down to BOND ING: a“Quartz” Wafer with bio-sensors on it TO a Silicon Wafer supporting both microprocessor and a radio emitter which means BONDING a wafer of Silicon Oxide , SiO 2 (= glass) to a Silicon wafer called Si(100) because of its “facet” => We are really researching Direct Nanobonding Between Si(100) and SiO 2 *
    • 30. Exploring Nano-Bonding of silicates and Si(100) wafers & dices
      • Goal – Direct Hermetic * bond between Si(100) and SiO 2 surfaces
      • Experimental Design
        • Wet Chemical Processing
        • Clamping
        • Annealing to induce bonding
      • Observation & Results
      • * Hermetic means NO LEAKING, NO CORROSION IN THE HUMAN BODY/SALINE SOLUTION !
    • 31. Let’s “NANO-bond!” = bond at the atomic scale, along crystal “facets” of the silicon crystal Silicon Wafer Quartz Wafer Silicon Wafer Quartz Wafer BEFORE AFTER
    • 32. SCIENTIFIC MOTIVATION: Understanding surface condensation , hydroaffinity, bonding at the nanoscale … How do water molecules interact with Si, SiO 2 ?
      • SiO 2 surfaces are very stable, hydrophobic
      • Etching creates dangling bonds on the SiO 2 surface,
      • renders hydrophilic
      • Si(100) is initially hydrophilic , very reactive
      • Our 6,613,677 patent passivates Si(100) with OH termination & renders it hydrophobic
    • 33. Wet Chemical Processing
      • Wet chemical processing (1) passivate or (2) make Si(100) and SiO 2 surfaces more reactive.
      • Herbots-Atluri process passivates Si(100) with OH-like groups (see ABOR US patent 6.616,677 (9/3/03)
      • Explore wet chemical processing to nucleate & grow nanophases across Si(100) /SiO 2 interfaces
      Passivated Si(100) Surface OH OH Reactive Surface OH OH
    • 34. Wet Chemical Processing of Si(100)
      • (1) Initial Native Oxide
      • (2) Hydrocarbon removal
      • (3) Aqueous HF etch
      • (4) Chemical oxide and planarization
      • (5) Oxide strip
      • (6) Silanol (OH) termination
        • Passivated but ready to react
      18 MegOhms Deionized (DI) Water rinse between each step for 10 minutes
    • 35. Polarization Properties
      • Contact Area Doubled in Size with NO Applied pressure
      • Polarization Due to Oxygen Deficient Oxide
      • Mixed Cleans Used to Maximize Effect
    • 36. Why Clamping?
      • Surface Roughness
        • 0.2 nm r.m.s
        • Terrace length > 20 nm
      • Warp
        • A+B < 30 microns
      • Thickness Variation
        • A+B < 25 microns
      • Herbots-Atluri clean smoothens surface from 2 nm to 20 nm terraces
      Clamped Surface
    • 37. 4. RESULTS: Two ASU Patents “Inhibition of condensation on surfaces ..” (Inter Occular Lenses (IOL’s, etc..)
      • Dr. Clive Sell, MD smiles as he applies our bio-compatible treatment, “VITREOX” to render an IOL hydrophilic.
      • He has used the technique successfully
    • 38. Motivation Scientific background
      • Understanding of Si and SiO 2 surfaces structure & properties
      • Silicon surface
        • After cleaning and passivation (inhibit further oxidation), dangling bonds are terminated resulting in hydrophobic behavior if the surface is “ordered”
        • Defects on the surface may act like nucleation sites for water condensation
      • Silicon with SiO 2 thin layer
        • Alter surface from hydrophobic to hydrophilic using Herbots-Aturi clean, then grow a SiO 2 thin layer
      • Demonstration of passivated, terminated, ordered Si(100) regions
      • Next to a defect rich Si(100) region
      • Using metered water drops for contact angle measurements to qualify (1) hydrophobic and (2) hydrophilic behaviors
    • 39. Motivation Scientific background
      • Model
        • Deposition of Si and O on a Si(100) substrate creates an SiO 2 thin layer
        • Silicon oxide reactive surface results in the hydrophilic behavior
      x y
    • 40. Outer Shell electrons (symbolized by ) Configuration available for bonding, defect (symbol for missing electron for a complete shell ) Building a Silicone Molecule Carbon has polymorphic phases, flexibility in bonds - + Oxygen Silicon Carbon Hydrogen More directional, single phase, only one kind of rigid bonding Strongly electronegative in the outer shell With 6 negatively charged electrons - Hydrogen is a strong electron donor
    • 41.
      • 2) Oxygen-Silicon-Oxygen-Silicon- Oxygen Atom Chain
      Method Model Silicone structure: SiO(CH 3 ) 2 is the building block (monomer) 1) First chemical building block Si-O atom pair 3) Si-O atom pair with electron configuration and bonding sites (a) Before bonding (b) After bonding 4) Backbone of the silicone chain Si-O-Si-O-Si-O-Si-O. showing the sites Available for bonding CH 3
    • 42. Method Model A Si-O chain with a CH 3 radical attached, the radical can rotate in the plane Defects and mobile charges Polydimethylsiloxane PDMS Silicone
    • 43.
        • Fogging = nucleation of water droplets + subsequent interaction to free mobile charges on hydrophobic surface
        • Ostwald ripening = droplets enlarges with time, small droplets combine to bigger droplets to minimize area to volume ratio & surface energy
      To Understand and inhibit condensation on Silicone surface
    • 44. Application Emergency device during retinal surgery Procedure Fogging DISTORTION Time to Fog (s) VitreOx™ NO NO > 1200 s (20 min) + Healon® YES YES 290 s Viscoat® YES YES 10 s Wiping YES YES 5 s Natural YES YES 3 s
    • 45. RESULTS ON DIFFERENT IOL’s Permanent coating on IOL devices Permanent Coating CONDENSATION DISTORSION Time to Time to Fog (seconds) Silicone IOL Preserved in air NO NO 1200 seconds + = 20 minutes + Silicone IOL Preserved in saline NO NO Ongoing Trials Hydrophobic acrylic IOL Preserved in saline NO NO Ongoing Trials
    • 46. 4. RESULTS: Two ASU Patents “Inhibition of condensation on surfaces ..” (Inter Occular Lenses (IOL’s, etc..)
      • Dr. Clive Sell, MD smiles as he applies our bio-compatible treatment, “VITREOX” to render an IOL hydrophilic.
      • He has used the technique successfully