Deplace, Fanny (2008) Waterborne Nanostructured Adhesives. PhD thesis Chimie et Physico-Chimie des Polymeres, Physico-Chimie des Polymères et Milieux Dispersés, ESPCI p.316.
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Abstract
We studied adhesive and deformation properties of soft polymer films made from nanostructured latex particles. A methodology based on two rheological criteria and suitable for all kinds of PSA has been proposed to optimize adhesive performances. It allowed us to identify strategies to improve the balance between adhesion and cohesion of PSA prepared from core-shell latex particles. An interesting strategy is the activation of an interparticle crosslinking reaction during the drying of the film. The heterogeneity of the network has been varied without changing the monomer composition. This crosslinking reaction has a spectacular effect on nonlinear properties of the materials. These properties are well described by a nonlinear model constructed from the combination of the Upper-Convected Maxwell model and the Gent model. Best results are obtained with PSA prepared from latex particles with a fine and crosslinked shell and a soft only slightly crosslinked core. With a more empirical approach, promising adhesive performances have been obtained with PSA prepared from in situ tackified latexes synthesized by miniemulsion polymerization.
Keywords: Adhesion, waterborne PSA, Latex particle, Heterogeneous structure, Linear viscoelasticity, Nonlinear viscoelasticity, Nonlinear elasticity.
| Item Type: | PhD Thesis (PhD) |
|---|---|
| PhD Supervisor: | Creton, Costantino |
| Date: | 11 April 2008 |
| Board of examiners: | Charleux, Bernadette and Gauthier, Catherine and Papon, Eric and Tassin, Jean-Francois and Derail, Christophe |
| Ecole Doctorale: | ED 397 PHYSIQUE ET CHIMIE DES MATERIAUX |
| Discipline: | Chimie et Physico-Chimie des Polymeres |
| Collection (Fonds): | ESPCI ParisTech |
| Institution: | ESPCI |
| Department: | Physico-Chimie des Polymères et Milieux Dispersés |
| Subjects: | 6. Chemistry, Physical Chemistry and Chemical Engineering |
| Uncontrolled Keywords: | Adhesion, waterborne PSA, Latex particle, Heterogeneous structure, Linear viscoelasticity, Nonlinear viscoelasticity, Nonlinear elasticity |
| ID Code: | 4244 |
| Deposited By: | Fanny Deplace |
| Deposited On: | 22 October 2008 |
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Table of content
List of Abbreviations 15
Introduction Générale 17
1. Theoretical Concepts 21
1.1. Polymers 25
1.2. Polymerization 29
1.2.1. FREE RADICAL CHAIN POLYMERIZATION 29
1.2.2. BRANCHED AND CROSSLINKED POLYMER FORMATION 32
1.2.2.1. Branched polymer formation 32
1.2.2.2. Crosslinked polymer formation 34
1.3. Some polymer analytical characteristics 35
1.3.1. AVERAGE MOLECULAR WEIGHT 35
1.3.2. FRACTION OF GEL 36
1.3.3. GLASS TRANSITION TEMPERATURE 37
1.4. Waterborne polymers 39
1.4.1. CONVENTIONAL EMULSION POLYMERIZATION 39
1.4.1.1. Batch emulsion polymerization 39
1.4.1.2. Semi-continuous emulsion polymerization 44
1.4.2. MINIEMULSION POLYMERIZATION 46
1.4.3. LATEX CHARACTERIZATION TECHNIQUES 48
1.4.3.1. Particle size 48
1.4.3.2. Solid content and viscosity 48
1.5. Film formation from the colloidal particles of the latex 49
1.5.1. FILM FORMATION MECHANISM 49
1.5.2. DRYING OF CORE-SHELL LATEX PARTICLES 54
1.6. Elasticity and Viscoelasticity 55
1.6.1. ELASTICITY 55
1.6.1.1. Thermodynamics of elastomer deformation 55
1.6.1.2. Statistics of ideal rubber elasticity 57
1.6.1.3. Mooney Rivlin phenomenological model 60
1.6.1.4. Gent phenomenological model 61
1.6.2. VISCOELASTICITY 64
1.6.2.1. Linear viscoelasticity 65
1.6.2.2. Linear viscoelastic phenomenological models 68
1.6.2.3. Nonlinear differential model: Upper Convected Maxwell model 71
1.7. Theoretical concepts of adhesion 79
1.7.1. TACK EXPERIMENTS 79
1.7.2. PREDICTION OF DEBONDING MECHANISMS FROM LINEAR RHEOLOGICAL PROPERTIES 84
2. State of the Art 89
2.1. Adjustable parameters during wb-PSA synthesis 93
2.2. Adhesive performance of wb-PSA 95
2.2.1. ADHESION CHARACTERIZATION TECHNIQUES 95
2.2.2. EFFECT OF REACTION COMPONENTS 99
2.2.3. EFFECT OF THE POLYMERIZATION PROCESS AND STRUCTURE 104
2.3. Conclusion 107
3. Experimental Techniques 111
3.1. Adhesive layer characterization: AFM technique 115
3.2. Adhesive properties 117
3.2.1. STANDARD INDUSTRIAL ADHESIVE TESTS 117
3.2.2. PROBE TACK TEST 118
3.2.3. POSSIBLE PREDICTIONS OF PEEL AND SHEAR FROM TACK RESULTS 124
3.3. Linear rheological properties 127
3.4. Tensile tests 135
4. From Structure to Properties 139
4.1. Introduction 143
4.2. Theoretical background 145
4.2.1. PREDICTION OF DEBONDING MECHANISMS FROM LINEAR RHEOLOGICAL PROPERTIES 145
4.2.2. PREDICTION OF DEBONDING MECHANISMS FROM NONLINEAR RHEOLOGICAL PROPERTIES 146
4.3. Materials 151
4.4. Particle and polymer design for adhesive properties 155
4.4.1. LINEAR VISCOELASTIC PROPERTIES AND ADHESIVE PROPERTIES 155
4.4.1.1. Influence of the elastic modulus: the PSA must be soft enough 155
4.4.1.2. Influence of the dissipative properties: how to further increase the adhesive energy 158
4.4.2. USE OF LARGE STRAIN DEFORMATION TO FURTHER REFINE PARTICLE DESIGN FOR ADHESIVE PROPERTIES 161
4.4.2.1. Activation of crosslinking at the interface of soft and dissipative particles: from a viscoelastic liquid to a viscoelastic solid 161
4.4.2.2. Influence of gel content and Mw of the sol of the core 163
4.4.2.3. Comparison between a viscoelastic material and a more elastic one 165
4.4.3. A MORE COMPLEX EXAMPLE 166
4.5. Conclusion 169
5. Role of the Interfaces on the Large Strain Behavior 173
5.1. Introduction 177
5.2. Experimental sections 181
5.2.1. MATERIALS 181
5.2.1.1. Synthesis description 181
5.2.1.2. System for the study of the effect of the crosslinks distribution 182
5.2.1.3. System for the study of the effect of an increase in crosslinking density 183
5.2.1.4. Additional remarks 184
5.2.2. STRUCTURE OF THE FILMS 185
5.2.3. ANALYSIS OF LARGE STRAIN BEHAVIOR 187
5.2.3.1. Elastic modeling 187
5.2.3.2. Viscoelastic / Hardening parallel model 187
5.2.3.3. Intermediate strain energy dissipation 194
5.3. Results and discussion 195
5.3.1. ACTIVATION OF THE CROSSLINKING REACTION 195
5.3.1.1. Adhesive performance 195
5.3.1.2. Linear viscoelastic properties 200
5.3.1.3. Extension to large strains 202
a. Elastic Mooney representation 203
b. Viscoelastic-hardening description 205
c. Intermediate strain dissipation 207
d. Comments on elastic vs. viscoelastic-hardening desriptions and intermediate strain dissipation 207
5.3.1.4. Rheological properties vs. adhesion 209
5.3.2. EFFECT OF THE DISTRIBUTION OF THE CROSSLINKING POINTS 211
5.3.2.1. Experimental results 211
a. Adhesive performance 211
b. Tensile results 216
5.3.2.2. Discussion 218
a. Molecular interpretations of the deformation behavior 218
b. Effect of rheology on adhesive properties 224
5.3.3. HOW TO FURTHER IMPROVE ADHESIVE PERFORMANCE: RESULTS ON MORE COMPLEX SYSTEMS 227
5.3.3.1. Increase in the gel content of the shell (less CTA in the shell) 227
5.3.3.2. Increase in the gel content of the core (less CTA in the core) 229
5.3.3.3. Effect of DAAM content in the shell 232
5.4. Conclusion 237
APPENDICES 238
6. Tackified wb-PSA synthesized by Miniemulsion 243
6.1. Introduction 247
6.1.1. BRIEF STATE OF THE ART OF TACKIFIER IN PSA FORMULATIONS 247
6.1.2. TACKIFIED WATERBORNE PSA 247
6.2. Tackifying resins 251
6.2.1. MONOMERS AND POLYMERIZATION PROCESSES 251
6.2.1.1. Aliphatic / aromatic hydrocarbon resins 251
6.2.1.2. Polyterpene resins 252
6.2.2. ROLE OF A TACKIFYING RESIN IN PSA FORMULATIONS 253
6.3. Tackified wb-PSA: the materials 255
6.3.1. ONE STAGE IN-SITU MINIEMULSION TACKIFICATION 255
6.3.1.1. Synthesis process 255
6.3.1.2. Latexes monomer composition 256
6.3.1.3. Material characterization 257
a. Selection of the type of tackifier resin 257
b. Tackifier resin content 258
c. Further remarks 259
6.3.2. IN-SITU TACKIFIED CORE-SHELL LATEXES 261
6.3.2.1. Synthesis process 261
6.3.2.2. Latexes monomer composition 262
6.3.2.3. Material characterization 263
6.4. Optical quality and nanostructure of adhesive films 265
6.4.1. ADHESIVE FILM OPTICAL QUALITY 265
6.4.2. AFM CHARACTERIZATION 265
6.4.2.1. One stage tackified latexes 265
6.4.2.2. Two stage tackified latexes 268
6.5. Adhesive and Rheological Results 271
6.5.1. INFLUENCE OF THE TYPE OF TACKIFYING RESIN ON TACK RESULTS 271
6.5.2. FURTHER RESULTS OF MINIEMULSION WITH PICCOTAC 1095-N 273
6.5.2.1. Linear viscoelastic properties 273
6.5.2.2. Influence of tackifier content on tack results 274
6.5.3. IN-SITU TACKIFIED CORE-SHELL LATEXES 276
6.5.3.1. In-situ tackified core-shell latexes vs. non tackified latex 276
a. Linear rheological properties 276
b. Tack results 277
6.5.3.2. Homogeneous vs. core-shell tackified latexes 278
a. Linear rheological properties 278
b. Tack results 279
6.5.3.3. Influence of the tackifier content of two stage latexes 280
6.5.3.4. Nonlinear deformation behavior 282
6.5.3.5. Core and shell optimization 284
6.6. Technical feasibility 287
6.7. Discussion 291
6.8. Conclusion 293
Conclusion Générale 297
Extended Abstract in French 301
Bibliography 311
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