Stoichiometric (Percentage) Calculations: Objective of Research Research Methodology Course Work Details

Ceramic Polymer Interface Development
Objective of Research
Research Methodology Material Description and Technique used Course Work Details
Stoichiometric (Percentage) Calculations

Symbol Meaning How to prepare
Percentage by mass
( ) 100 ( ) ( ) 100 ( )
5%: Dissolve 5 g of solute in 95 g solvent 5%: Dissolve 5 g of solute in 100 mL of solution 5M: Dissolve 5 mol of solute in solvent and add solvent to make 1L of solution 5m: Dissolve 5 mol of solute in 1 kg of solvent
Percentage by volume
Molarity
Molality
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Polymer Selection:
Structure of Epoxy resin Structure of DETA
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Polymer Selection:
O NH2 NH2
CH3
O
O
O
CH3
NH2
NH2
OH NH2 N H CH2 O
CH3
OH O CH2 N H NH2
CH3
Most of the epoxy resins that are used in the formulation of adhesives have EEWs in the range of 180 to 3200, corresponding to a molecular weight range from 250 to 3750.
Ref: Mechanical Engineering Hand Book: Lehman, R.L.; et. al. Materials
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The structure and properties of epoxy resin
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Structure of DGEBA:
n = degree of polymerization Epoxy Equivalent weight (EEW): de g
Amine Hydrogen Equivalent Weight: Diethylenetriamine (DETA) Triethylenetriamine (TETA)
Amine functionality = 4
Amine functionality = 6
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Example of Stoichiometric Calculation: Resin: DGEBA Amine Curing Agent: Triethylene Tetramine (TETA) Molecular Weight of Amine: 6 carbons 4 nitrogents 18 hydrogens Molecular Weight = 6 x12 = 72 (g/mol) = 4 x14 = 56 (g/mol) = 18 x1 = 18 (g/mol) = 146 (g/mol)
There are 6 amine hydrogen functionally reactive with an epoxy group Therefore
146( ) = 24.3 6( )
Thus, 24.3 grams of TETA are used per equivalent of epoxy. If the DGEBA has an equivalent weight of 190 (380 g/mol/2 eq./mol), then 24.3 grams of TETA are used with190 grams of DGEBA, or 24.3/190 13 grams of TETA per hundred grams of DGEBA. Mallikarjunachari.G Date: 15/02/2013 1/3

Hysteresis 1. Mechanical Hysteresis surface roughness
2. Chemical Hysteresis Parameters affect the contact angle 1. Temperature
2. Material Transitions Eg: glass and crystalline transitions, contaminants and adsorbed materials polar and apolar interactions, drop dimension, surface crystallinity, molecular weight and conformation of chains.
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Hysteresis 1. Mechanical Hysteresis surface roughness Acid Base interactions ( Exothermic Reaction)
2. Chemical Hysteresis
Parameters affect the contact angle

1. 2. 3. 4. 5. Temperature Gravity Relative Humidity Porosity Surface Roughness
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Literature
EFFECTS OF STOICHIOMETRY AND EPOXY MOLECULAR MASS ON WETTABILITY AND INTERFACIAL MICROSTRUCTURES OF AMINE-CURED EPOXIES
Epoxy Equiv. Mass (g/mol)
degree
degree
Surface free energy components (mJ/m2) 36.88 40.40 36.32 35.28 35.30 35.17
53.85 58.45 52.13 55.03 53.39 52.98
190 255 500 900 2250 3050
63.10.7 59.31.6 65.71.4 58.51.5 61.71.9 62.31.6
40.61.3 32.14.2 41.91.8 44.11.3 44.11.1 44.41.2
16.97 18.05 15.80 19.74 18.08 17.81
, water and methylene iodine contact angle respectively, , , : Nonpolar, polar and total surface free energy, respectively. Values after the sign indicate one standard deviation. Conclusion: Epoxy molecular mass does not seem to affect wettability of amine cured epoxies Mallikarjunachari.G Date: 15/02/2013 1/3

Literature: The contact angle of thin-uncured epoxy lms: thickness effect Materials: Double Distilled water, diiodomethane and glycerine
Coating Thickness range: 5-75 nm
Film formation: Spin coating Speed : 2000 to 4000 rpm
Substrate: Dia: silicon wafer 5cm Thickness : 150 nm
Thickness Measurement: Micro spectrophotometer
Contact Angle Measurements & Conditions: Kruss G40 At temp: 20oC, After 1 min, Size of droplet: 10 ml for water 5ml for methylene diode
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Literature: The contact angle of thin-uncured epoxy lms: thickness effect
Fig. Surface tension of epoxy lm with different thicknesses on oxidized silicon wafers, calculated by LW/AB and harmonic mean method.
Fig. Surface tension based on harmonic mean method and their components vs. thickness.
Conclusion: The results show that the nature of the surface of epoxy films change to more hydrophobic state as its thickness increases Mallikarjunachari.G Date: 15/02/2013 1/3

Literature: The contact angle of thin-uncured epoxy lms: thickness effect Contact Angle of EG and and MI on a thin film Liquid Time (min) 1 MI EG 43.1 46.1 5 40.5 46.7 10 32.8 45 15 30.4 47.1 20 26.8 45.2 25 25.4 46.9
Contact Angle of MI on a thick film Time (min) 1 2 3 4 5 MI 25.7 18 14.4 7.9 vanish
Contact Angle of EG and on a thick film Time (min) 1 EG 60
5
10 20 25
56.5
55.3 54.1 51.3
Conclusion: The results show that the nature of the surface of epoxy films change to more hydrophobic state as its thickness increases Mallikarjunachari.G Date: 15/02/2013 1/3

MD Simulations: Research Methodology Material Description and Technique used Course Work Details
Ref: Effects of temperature, size of water droplets, and surface roughness on nanowetting properties investigated using molecular dynamics simulation
Effect of Temperature:
Fig. Snapshots of the spreading process of water droplets with time for various temperatures. The colors of atoms in the droplet represent the magnitude of internal energy.
Fig. Variation of the dynamic contact angle of a water droplet on the Au substrate with time for temperatures of 250400 K.
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Fig. 3. Variation of average internal energy per water molecule with time for temperatures of 250400 K.
Fig. 5. Radical distribution function of a water droplet on the Au substrate for temperatures of 250400 K.
Effect of drop size:
Fig. Snapshots of the spreading process of water droplets with time at room temperature. The initial diameters of water droplets are 4.5, 6.0, and 7.5 nm, respectively. The colors of the atoms in the droplet represent the magnitude of slip vectors.
Fig. 8. Relationship between dynamic contact angle and (a) time and (b) spreading area. The initial diameters of droplets are 4.57.5 nm.
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Fig. 8. Relationship between dynamic contact angle and (a) time and (b) spreading area. The initial diameters of droplets are 4.57.5 nm.
Fig. Variation of average internal energy per water molecule with time. The initial diameters of droplets are 4.57.5 nm.
Fig. Radial distribution function of a water droplet on the Au substrate. The initial diameters of droplets are 4.57.5 nm.
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Effect of surface roughness:
Fig. Snapshots of the spreading process of a water droplet with time at room temperature for substrates with Ra = (a) 0, (b) 0.58 and (c) 0.86 nm. The colors of the atoms in the droplet represent the magnitude of slip vectors.
Fig. Radial distribution function of a water droplet on the Au substrate for substrates with Ra = 0, 0.58, and 0.86 nm.
Fig. Variation of the average internal energy per water molecule with time for substrates with Ra = 0, 0.58, and 0.86 nm.
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Nanoscratching of Metallic Thin Films on Silicon Substrate: a Molecular Dynamics Study
Fig. Changes in atomic arrangement during nanoscratch test for Al-Si sample. The horizontal and vertical loads are 80 and 37.5 nN, respectively. The durations are (a) 0.0, (b) 2.1, (c) 4.2 and (d) 6.3 ps.
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Fig. Height of indentor under each load during simulation of Al-Si samples. The height is measured on the basis of the interface between the substrate and the thin lm.
Fig. Pressure of the contact area for Al-Si samples. Average pressures for 35, 37.5, and 40 nN vertical loads are 15.80, 12.89, and 9.82 GPa, respectively.
Fig. Maximum friction constant in the nal stage of scratching for Al-Si samples as a function of vertical load.
Fig. Comparison of critical load for lm failure (gray bars) and the interface energy of heterogeneous junction (black bars) for each sample. The critical load is detected with the maximum friction constant, and the interface energy is calculated as the potential energy difference between the separated and adhesion states.
Fig. Comparison of maximum friction constant (gray bars) and interface energy of heterogeneous junction (black bars) for each sample.
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Sources of Thermodynamic Contact Angle Hysteresis General Assumption

Surface is smooth
Specific Assumption
Surface must be smooth at the 0.1 to 0.5 m level Surface must be homogeneous at the 0.1 m level and above
Effect on Hysteresis
increase with increasing roughness (adv. increases and rec decreases with increasing roughness) adv. dependent on low energy phase: rec dependent on high energy phase
Time Dependent
No
Surface is homogeneous
No
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Sources of Kinetic Contact Angle Hysteresis General Assumption

Surface is nondeformable Wetting liquid does not penetrate surface Surface does not reorient Surface immobile, therefore, surface entropy is constant
Specific Assumption
Modulus of elasticity in surface > 3x105 dyne/cm Liquid molecular volume > 60-70 ccmole Reorientation time at time of measurement Configurational entropy independent of local environment
Effect on Hysteresis
Not known
Time Dependent
Yes due to surface deformation/relaxation effects Yes due manly to diffusion
Increased liquid penetration lends to increased hysteresis
Increased tendency to orient lends to increased hysteresis Unknown but probably increase in hysteresis as surface mobility increases
Yes
Yes
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Work of Adhesion, Critical Load and Nanoscratch Progressive Load scratch Test
Critical Load:
Common radii are from 20 to 200m for micro/macro scratch tests, and 1 to 20m for nano scratch tests.
Definition: When performing a progressive load test, the critical load is defined as the smallest load at
which a recognizable failure occurs. In the case of a constant load test, the critical load corresponds to the load at which a regular occurrence of such failure along the track is observed.
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Critical Load
Figure : Micrograph of Failure Tin Coating 500x magnification (image width 0.0615mm)
Test Parameters
Load type Initial Load Final Load Loading rate Progressive 0.015 mN 20.00 mN 20.00 mN/min Critical Loads Tin Coating Scratch 1 2 Failure (mN) 40.152 42.242
Scratch Length
Scratching speed, dx/dt Indenter geometry Indenter tip radius Indenter material (tip)
1.6 mm
1.601 mm/min 90 conical 2 m Diamond
3
4 5 Avg Value Stnd Deviation
42.217
41.293 40.992 41.379 0.882
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Parameters Effecting Critical Load
A Study of Adhesion of Silicon Dioxide on Polymeric Substrates for Optoelectronic Applications
Fig. Scratch test curve of SiO2 layer of untreated AryLiteTM with optical image in the plot inset (magnification 20x)
Fig. Scratch test curve of SiO2 layer of treated AryLiteTM with optical image in the plot inset (magnification 20x). Topography and scratch scan refers to the third wear
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Parameters Effecting Critical Load
The test specific parameters include 1. Loading Rate 2. Scratching Speed 3. Indenter tip radius 4.Indenter Material
The sample specific parameters include 1. Friction coefficient between surface and indenter 2.Internal stresses in the material for bulk materials
3. Material hardness and roughness For coating-substrate systems

4. Substrate hardness and roughness 5. Coating hardness and roughness 6. Coating thickness
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Scratch Models Model I Benjamin and Weaver: They proposed two scratch models based on (a) tangential force (Fx) at the tip and (b) normal force. The 1st model can be summarized as:
3 2 = + + 12 4
where, d is scratch width, R is the tip radius, Hs and Hc are the hardness of substrate and coating, respectively; is the shear stress at the coating substrate interface and t is the thickness of the coating. The 1st , 2nd, and 3rd terms in the RHS of the equation are the ploughing force required to deform the substrate, the force to remove coating from the surface, and the ploughing force required to push aside the sheared film, respectively. This model can be used to obtain critical shear stress (tc) of the coating-substrate interface. This model was found to work well with Al-coated glass specimen.
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Scratch Models Model II Benjamin and Weaver:
(2 2
where, a is the contact radius between the tip and the coating (a d/2).
The model gives a measure of adhesion in terms of critical shear stress by substituting a measured at the critical load. Ollivier and Matthews:
2 (2
where, Lc = critical load and ac = contact radius at the critical load.
This model was able to yield semi-quantitative results for DLC films.
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Scratch Models Model IiI Laugier: Total compressive stress (x) under the leading edge of the indenter is expressed as
3 * = 4 + (1 2 ) 22 8
where, is the Poissons ratio of the substrate and is friction coefficient (Fx/Fz) between the indenter and the coating.
The first terms originates from the compressive stress at the leading edge of the indenter induced by the friction during sliding. The second term describes the radial surface stress at the edge of the contact circle induced by the force normal to the surface. Assuming elastic Hertzian contact, the contact radius (a) is expressed as:
2 2 3 1 1 = ( + 4
is the Poissons ratio of the coating, Es and Ec are the Youngs moduli of the substrate and the coating, respectively.
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Scratch Models Model II For a << R, the shear stress () acting on the coating-substrate interface at the lip of the indentation was approximated as :
The value of the at the critical load is considered a measure of coating adhesion. Laugier later introduced
practical work on adhesion (W) as:

2 = 2
The critical stress ( ) is the sum of external stress and internal stress at the critical load. This model was purely elastic, and it was assumed that a >> t. The model predicted results on carbide and nitride coatings reasonably.
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Scratch Models Model IV
Burnett and Rickerby: The driving forces for removal of coating consists of components of (i) an elastic-plastic indentation stress, (ii) an internal stress, and (iii) tangential force. The following relation was derived for critical scratching load:
2 2 = 8
0.5
where, W is the work of adhesion, dc is the scratch width at the critical load.
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Scratch Models Modified Model Bull et al [7] modified Burnett-Rickerby model assuming that the coating detachment occurs when the tangential compressive stresses in the coating in front of the stylus induce critical tensile stresses normal to the coating-substrate interface: The critical load is given by:
2 =
0.5
This Equation could be used to calculate work of adhesion (W).
where Ac is the cross-sectional area of the scratch track at the critical load:
2 = 2 sin1 ( ) 2 2 2
2 0.5
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Scratch Models Limitations: 1. The existing models invariably use assumptions and simplifications to deal with the inherent complexity of any scratching process, which involves large number of variables. Hence, the existing scratch models experience great difficulties to give a complete analytical description of the mechanics of scratch testing. Predicted scratch adhesion values from such models differ widely from the actual scratch test results. Evaluation and fine-tuning of such scratch models certainly requires continuous developmental effort with an objective to obtain a standard model that would give comprehensive description of any scratching process
2.
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Objective and Plan
Epoxy Curing
Surface Energy Based on Contact Angle
1. 2. 3. Surface Roughness Chemical inhomogeneity Rapid Conformational Changes
(DGEBA + DETA)
State 1
State 2
State 3
State 4
Thin Film Coating based on interaction energy

1. 2. 3. High surface Energy Intermediate Energy Lower Energy
P1 P2 P3
P1 P2 P3
P1 P2 P3
1
P1 P2 P3
1
Critical Load
1. 2. Thickness Measurement Work of Adhesion Measurement
5 Scratch + 5 Microscopy 5 Scratch + 5 Microscopy 5 Scratch + 5 Microscopy
5 scratch + 5 Microscopy 5 scratch + 5 Microscopy
5 scratch + 5 Microscopy
5 scratch + 5 Microscopy 5 scratch + 5 Microscopy 5 scratch + 5 Microscopy
Total
1. 2.
60 scratch tests 60 Microscopy tests
Without Knowing Science
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S.No.
Solid Polymer
Surface free energy (SFE) at 20 C in mN/m 45.0

46.5( Tg = 60) 40.2(100)
CAS no
Price (Rs)
1
2 3
Polyvinylidene chloride PVDC

Polyamide (Thermoset) PMMA(Thermoplastic) Polytetrafluoroethylene (Teflon) Polystyrene
9002-85-1
32131-17-2 87210-32-0
22433.10 250 grams 12503.46 100 grams
4
5
19(130)
42(100)
9002-84-0
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Adhesion of polymerinorganic interfaces by nanoindentation
Geometry: Glass dimension - 1 mm3 PS -660nm PMMA 1.5 m Method: Spin Coating Equipment: Micromechanical Tester Loads: 250
Purpose of PMMA is to promote the adhesion between Glass and Polystyrene
FIG. Contact AFM: (a) deflection image; (b) height image; (c) cross-sectional trace of an indent corresponding to 10-mN peak load.
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FIG. Indentation-induced delamination: (a) deflection image; (b) height image; (c) cross-sectional trace. The contact and delamination diameters are 2a and 2c, respectively.
FIG. Topography of the fracture surface on the substrate side underneath the delaminated film shown in Fig. 3(a)(c) are deflection, height, and friction images, respectively. (d) is a schematic of the crack arrest mark formed by polymer beads.
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Quantitative adhesion measures of multilayer films: Part II. Indentation of W/Cu, W/W, Cr/W
Without super layer
With super layer
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Measurement of adherence of residually stressed thin films by indentation. I. Mechanics of interface delamination
FIG. Schematic of indentation-induced delamination at the interface of a thin fihn and substrate.
Buckling Shapes Mallikarjunachari.G
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Method Concept
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If G value is more adhesion is more As expected, higher value of surface energy increases the critical stress whereas a longer crack reduces it. Larger modulus means that the plate is capable of storing less energy resulting into smaller energy release which, in turn, requires higher stress for making the crack critical If G value is less is stronger interface. Good adhesion. If surface energy is more G value is less is less. Work of Adhesion is more then G value is less or Good adhesion which needs more stress finally less bulging or delamination.
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Contact angles in of standard liquids on various polished cement paste surfaces Materials OPC 0.3 OPC 0.5 BC 0.5 Diiodomethane Ethylene glycol Formamide Glycerol
14 2 14 3 23 4
18 4 16 2 17 4
18 2 18 2 19 2
30 3 24 2 26 4
OPC Ordinary Portland Cement BC Blended cement Surface Energy Components (mJ/m2) of the various cement pastes, as determined using the owens and wendt approach Materials OPC 0.3 OPC 0.5 BC 0.5 Mallikarjunachari.G
42.2 43.0 41.2
11.9 15.8 16.5

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57.1 58.8 57.7

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Fracture Toughness: Influencing Parameters: Extrinsic variables: Film thickness, extent of delamination, thickness and temperature Intrinsic ones are modulus, yield strength, the thermodynamic work of adhesion
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S.No. 1
Polymer PMMA
solvent
Spin speed
Thickness
2
3 4 5
PVP
POLYETHYLENE POLYSTYRENE TEFLON
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PMMA thin film preparation
Solvent - Dichloroethane
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POPYSTYRENE thin film preparation
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TEFLON thin film preparation
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Stoichiometric (Percentage) Calculations: Objective of Research Research Methodology Course Work Details

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Ceramic Polymer Interface Development