CHIMICA DELLE SUPERFICI ED INTERFASI
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1 CHIMICA DELLE SUPERFICI ED INTERFASI DOTT. GIULIA FIORAVANTI UNIVERSITÀ DEGLI STUDI DELL AQUILA LAUREA MAGISTRALE IN INGEGNERIA CHIMICA A.A
2 OUTLINE SURFACE CHEMICAL GRADIENTS DROPLET MOVEMENT ON WETTABILITY GRADIENT WETTABILITY GRADIENT FORMATION SILANES GRADIENT ON SI THIOLS GRADIENT ON AU BY WITHDRAWING EC DESORPTION Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 2
3 SURFACE GRADIENTS PROPERTIES THE SURFACE PHYSICAL AND CHEMICAL PROPERTIES CHANGE CONTINUOUSLY ALONG THE MATERIALS. PHYSICOCHEMICAL NATURE DIMENSIONALITY (1D, 2D, 3D) DIRECTIONALITY (UNIDIRECTIONAL, ORTHOGONAL OR RADIAL) LENGTH SCALE (CONTINUOUS OR DISCONTINUOUS) TEMPORAL DEPENDENCY (STATICAL OR DYNAMICAL) FUNCTIONALITY Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 3
4 SURFACE GRADIENTS Surface Gradients Attributes Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 4 Genzer et al. 2008, Langmuir, 24,
5 SURFACE-CHEMICAL GRADIENT APPLICATIONS SMART RESPONSIVE MATERIALS DRIVING RECORDING SCREENING (PHYSICOCHEMICAL PHENOMENA) BIOLOGYCAL APPLICATIONS CELL ADHESION PROTEIN ADSORPTION CELL GROWTH Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 5
6 SURFACES BIOFUNCTIONALIZATION Protein «Click Chemistry» Protein Protein Streptavidin D-Biotin N 3 - N N N SAM Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 6
7 WETTABILITY GRADIENT CHEMICAL HETEROGENEITY AND SURFACE ROUGHNESS (MICRO/ NANO SCALE) Superhydrophobic surfaces Lotus leaf effect Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 7
8 DUE TO WETTABILITY GRADIENT!!! MAIN GOAL: DROPLETS MOVEMENT Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 8
9 BENZYLIC AMIDE ROTAXANES Teflon Nature Mat., 2005, 4, 704 Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 9
10 TRANSPORT ON SURFACE UV-LIGHT ISOMERIZES THE FUMARAMIDE STATION, CAUSING THE DISPLACEMENT OF THE MACROCYCLE, WHICH CONCEAL THE FLUOROALKANE UNITS LEAVING A MORE POLAROPHILIC SURFACE Nature Mat., 2005, 4, 704 Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 10
11 SURFACE-CHEMICAL GRADIENT PREPARATION TECHNIQUES Technique Adsorbate Substrate Diffusion Printing Advancing solution Vapour phase Silanes Si, PDMS Solvent Silanes Si Through a matrix Alkanethiols, Silanes Au Contact Alkanethiols, Silanes Au, Si (also functionalized) Ink jet Alkanethiols, Silanes Au, Si Concentration gradient Monomers, Proteins Au, Si (also functionalized) Controlling reaction time Alkanethiols, Silanes Au, Si Depletion Proteins PDMS, Glass Irradiation Intensity, exposure time, mask Silanes, Alkanethiols, Monomers, Proteins Controlled polymerization Temperature, plasma or electropolymerization Alkanethiols, Monomers Au, Si (also functionalized) Desorption By potential or irradiation Alkanethiols Au Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 11 Au
12 WETTABILITY GRADIENT BY MIXED SAM APPROACH Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 12
13 WHAT MEANS "MIXED SAM"? TWO DIFFERENT FUNCTIONALITY (HYDROPHOBIC, HYDROPHILIC) WITH DIFFERENT DENSITIES ALONG THE SURFACE. Head group = CH 3 Head group = COOH Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 13
14 MIXED SAM FORMATION 1. KINETIC CONTROL: THE MOLECULES IN SOLUTION REACH RANDOMLY THE METAL SURFACE AND BIND IRREVERSIBLY TO IT. THE RESULT OF THIS PROCESS LEADS TO THE FORMATION OF AN ORGANIC MATRIX IN WHICH THE TWO COMPONENTS ARE ARRANGED RANDOMLY, IN SUCH PROPORTION AS TO REFLECT THE COMPOSITION OF THE STARTING SOLUTION. 2. DIFFUSION MECHANISM: THE IRREVERSIBLE CHEMISORPTION IS FOLLOWED BY A DIFFUSION AT THE SURFACE WHICH RESULTS IN A REDISTRIBUTION OF THE ADSORBATES, TO GIVE A FINAL SITUATION IN WHICH THEY ARE ARRANGED IN THE WAY THAT BEST SUITS THEM (ALBEIT LIMITED BY THE CONSTRAINTS IMPOSED BY THE KINETIC PHASE INITIAL ADSORPTION). Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 14
15 MIXED SAM FORMATION 3. EXCHANGE MECHANISM: ADSORPTION IS NOT AN IRREVERSIBLE PROCESS, BUT A DYNAMIC ONE: AFTER A FIRST STATISTICS ARRANGEMENT, THE CONTINUOUS PROCESSES OF ADSORPTION AND DESORPTION REQUIRE ACHIEVEMENT OF A FINAL THERMODYNAMIC EQUILIBRIUM, GENERALLY REPRESENTED BY THE FORMATION OF DOMAINS OF MOLECULES OF THE SAME KIND. Two sequential STM images taken 37 min apart showing a SAM containing islands of CH 3 (CH 2 ) 15 S- (topographically lower, shown as darker) surrounded by CH 3 OCO(CH 2 ) 15 S- (topographically higher, shown as brighter) areas. The SAM was formed from a solution of 75% CH 3 OCO(CH 2 ) 15 SH/25% CH 3 (CH 2 ) 15 SH on Au{111}. Domain coalescence is observed at this time scale (indicated by the two arrows). The reverse process (one large domain separating into two smaller ones) was not observed. Stranick et al., J. Phys. Chem. 1994,98, Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 15
16 MIXED SAM FORMATION SIMULTANEOUS DEPOSITION VERSUS CONTROLLED DEPOSITION. TYPICALLY, SOLUTION PROCESSING AND THE SAME ANCHOR CHEMISTRY ENABLE FULL CONTROL OF THE SAM COMPOSITION, WHICH DIRECTLY RELATES TO THE STOICHIOMETRIC COMPOSITION OF THE SOLUTION. Water contact angles measured on a self-assembled monolayer (SAM) of 100% alkyl phosphonic acid (a), on a mixed SAM of 50% alkyl and 50% fluoroalkyl phosphonic acid (b), and on a SAM of 100% fluoroalkyl phosphonic acid Zschieschang et al, Adv. Mater. 2010, 22, Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 16
17 CONTROLLED ADSORPTION 1 TWO-STEP IMMERSION METHOD THE FIRST IMMERSION (OR EMERSION) IS PERFORMED BY USING A LINEAR MOTION DRIVE. 1. LINEAR MOTOR 2 2. SAMPLE HOLDER 3. SAMPLE 3 4. ADSORBATE SOLUTION 1 4 Morgenthaler et al. 2003, Langmuir, 19(25), Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 17
18 CONTROLLED ADSORPTION DIPPING OR UNDIPPING STRATEGY (ADSORBATE 1) Thiols / Au Silanes / Si Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 18
19 SECOND STEP PARTIAL MONOLAYER FULL MONOLAYER (COMPLEMENTARY SAM) THE SUBSTRATE WAS IMMERSED IN A SOLUTION CONTAINING ADSORBATE 2. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 19
20 SAM COMPLEMENTARI Substrate Adsorbate 1 Type Adsorbate 2 Type Au Si CH 3 thiol Dodecanthiol OH thiol CH 3 thiol Dodecanthiol COOH thiol CH 3 silane Perfluoro silane Octadecyltrichlorosilane or Butyltrichlorosilane Trichloro(1H,1H,2H,2H PerfluoroOctyl)Silane NH 2 silane 11-Mercapto-1- Undecanthiol 11-Mercapto Undecanoic acid - - Aminopropyl Triethoxysilane (APTES) VARIABLES: - THIOLS/SILANES CONCENTRATION - SPEED OF WITHDRAWAL/DIPPING Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 20
21 CARATTERIZZAZIONE CONTACT ANGLE MEASUREMENTS (WATER) Au SUBSTRATE/THIOLS Item 1: [CH 3 ] = 10-3 mm; [OH] = 10-2 mm; speed = 20 µm/s Item 2: [CH 3 ] = 1 mm; [OH] = 10-2 mm; speed = 40 µm/s Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 21
22 RELATED OBSERVATIONS FULL COVERAGE OF MIXED THIOLS ON AU INFLUENCE OF ADSORBATE 1 CONCENTRATION (CH 3 ) LITTLE INFLUENCE OF ADSORBATE 2 INFLUENCE OF LINEAR MOTOR SPEED (PARTIAL MONOLAYER) NOT MARKED WETTABILITY GRADIENT (NO DROPLETS MOVEMENT) NOT FLAT SURFACE (AU DEPOSITED ON GLASS) PRELIMINARY RESULTS (REPRODUCIBLE) Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 22
23 SILANES ON SI SURFACES CONTACT ANGLE MEASUREMENTS (WATER) - Si SUBSTRATE/SILANES MONO: PERFLUORO OCTYLSILANE MIXED: PERFLUORO OCTYLSILANE + AMINOPROPYL TRIETHOXYSILANE Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 23
24 2µm AFM 2µm 2µm 2µm Bare Si 2µm 2µm Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 24 2µm
25 AFM CHARACTERIZATION High coverage c) Zone 3 b) Zone 2 a) Zone 1 Low coverage a. Typical AFM topography of zone 1 (bar 1.5 µm z scale 1 nm) b. Corresponding LFM image recorded with 1 nn load force after nanorubbing using 4 nn loading force in the central zone. c. Typical AFM topography of zone 3 (bar 1.5 µm z scale 1.5 nm) d. Corresponding LFM image of c. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 25
26 XPS CHARACTERIZATION Zone 3 High coverage XPS characterization: C1s and F1s evolution in the three regions of the wettability gradient. Zone 2 Zone 1 Low coverage Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 26
27 AFM CHARACTERIZATION Zone 3 High coverage Typical AFM images of silicon surface functionalized by TPOS corresponding to a a) zone 1 and b) zone 3 of the samples. Zone 2 Zone 1 Low coverage Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 27
28 SILANES ON SI SURFACES Static Water Contact Angle measurements along the gradient and exponential fit. Measurements at 25 C in air. TPOS Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 28
29 DROPLET MOVEMENT Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 29
30 DROPLET MOVEMENT a) Plot of the droplet position of the drop during the movement along the gradient. b) Images of the droplet in motion. The red arrows are proportional to the velocity of the movement. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 30
31 RELATED OBSERVATIONS MARKED SLOPE IN WETTABILITY GRADIENT ( ) DROPLETS MOVEMENT ( θ/ x > 10 )!!! SILANES COVERAGE CONFIRMED BY XPS ANALYSIS FLAT SURFACE USEFUL FOR LATERAL FORCE AFM (?) PROBLEMS IN REPRODUCIBILITY (?) PROBLEMS IN DYNAMIC CONTACT ANGLE MEASUREMENTS Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 31
32 WECD - WITHDRAWAL ELECTROCHEMICAL DESORPTION NEW TECHNIQUE DESORPTION WHILE WITHDRAWING THE SUBSTRATE APPLICABLE TO ANY METALLIC SURFACES COVERED BY THE PROPER ADSORBATE EASY AND REPRODUCIBLE Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 32
33 WECD - WITHDRAWAL ELECTROCHEMICAL DESORPTION FIRST STEP: FULL COVERAGE OF THIOLS (CH 3 ) ON AU SECOND STEP: CONTROLLED ELECTROCHEMICAL DESORPTION (PARTIAL COVERAGE) THIRD STEP: COMPLEMENTARY ADSORPTION (OH) Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 33
34 ELECTROCHEMICAL DESORPTION 0.5 M KOH solution in Millipore water Reference: Ag/AgCl Counter: Pt sheet Working: SAM covered surface Au-S-R + e - Au + R-S - Speed: 100 mv/s Cycling from a voltage of V to V, and then returning to V. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 34
35 ELECTROCHEMICAL DESORPTION Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 35
36 hydrophobic CONTACT ANGLE MEASUREMENTS hydrophilic Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 36
37 TIME DESORPTION And so on Speed = 100 mv/s; Reference electrode: Ag/AgCl; Counter electrode: Pt wire; Working electrode: SAM/Au. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 37
38 TIME DESORPTION - CV Solution: 0.5 M potassium hydroxide (KOH) and 5.0 mm of ferricyanide K 3 Fe(CN) 6 a) Repeated cyclic voltammetries from 1 to 9 cycles. b) Repeated cyclic voltammetries from cycle 10. Reference electrode: Ag/AgCl; Counter electrode: Pt wire; Working electrode: SAM/Au; 0.5 M potassium hydroxide (KOH) and 5.0 mm of potassium ferricyanide K 3 Fe(CN) 6 solution; Speed = 100 mv/s. Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 38
39 RELATED OBSERVATIONS FULL COVERAGE OF MIXED THIOLS ON AU INFLUENCE OF ADSORBATE 1 CONCENTRATION (CH3) LITTLE INFLUENCE OF ADSORBATE 2 INFLUENCE OF LINEAR MOTOR SPEED (PARTIAL MONOLAYER) NOT MARKED WETTABILITY GRADIENT (LITTLE DROPLETS MOVEMENT) NOT FLAT SURFACE (AU DEPOSITED ON GLASS) PRELIMINARY RESULTS (REPRODUCIBLES) Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 39
40 hydrophobic DROPLETS MOVEMENT ON SURFACE Solvent 1 Solvent 2 FINAL GOALS: DROPLETS ENCOUNTER hydrophilic CHEMICAL REACTION ON SURFACE Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 40
41 THE END!!! Corso di Chimica delle Superfici ed Interfasi - G. Fioravanti 41
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