Nondestructive testing of defects in adhesive joints

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In-situ generation of silica in epoxy matrix and modified epoxy matrix via solgel process K.K.Iynesh Kumar and B.Kothandaraman Department of Rubber and Plastics technology, Madras Institute of Technology, Anna University, Chennai, India. Email: iyneshkumar@gmail.com bkraman@mitindia.edu ABSTRACT The precipitation of nanosilica was done through Sol-Gel process with Tetraethoxysilane (TEOS) as silica precursor at room temperature. The choice of epoxy as a matrix was made because of its polar nature which can interact with in-situ generated silica. The amine containing polydimethylsiloxane (PDMS) was used as liquid rubber modifier. The precipitation was done directly on the organic matrix in the presence of Water, Tetraethoxysilane (TEOS) and Ethanol as mutual solvent. The nanocomposite was cured by triethylene tetramine at room temperature. To enhance bonding between organic and inorganic matrix Dichlorodimethylsilane (DDS) was used as a coupling agent. Dispersion of silica particles was observed through Atomic force microscope (AFM). Infrared spectroscopic studies indicated the occurrence of chemical interaction within the epoxy/silica under ambient conditions. The glass transition temperature (Tg) was investigated through Differential scanning calorimeter (DSC). The thermal stability and filler content of the material were predicted through Thermogravimetricanalyser (TGA). The mechanical reinforcement within the material was demonstrated through flexural behavior of the material. INTRODUCTION The sol-gel process, which is mainly based on inorganic polymerization reactions, is a chemical synthesis method initially used for the preparation of inorganic materials such as glasses and ceramics. Its unique low-temperature processing characteristic also provides unique opportunities to make pure and well-controlled composition organic/inorganic hybrid materials through the incorporation of low molecular weight and oligomeric/polymeric organic molecules with appropriate inorganic moieties at temperatures under which the organics can survive. The organic/inorganic hybrid materials made in this way, which have been termed “creamers” by Wilkes [1] and “ormosils” or” ormocers” by Schmidt[2]., are normally nanocomposites and have the potential for providing unique combinations of properties which cannot be attained by other materials . For the past decade, organic/inorganic nanocomposites prepared by the sol-gel process have attracted a great deal of attention, especially in the fields of ceramics, polymer chemistry, organic and inorganic chemistry, and physics. The preparation, characterization, and applications of organic/inorganic hybrid materials have become a fast expanding area of research in material science. The major driving forces behind the intense activities in this area are the new and different properties of the nanocomposites which the traditional macroscale composites and conventional materials don’t have. For example, unlike the traditional composite materials which have macroscale domain size of millimeter and even micrometer scale, most of the organic/inorganic hybrid materials are nanoscopic, with the physical
constraint of several nanometers, typically 1-100nm, as the minimum size of the components or phases. Therefore, they are often still optically transparent although microphase separation may exist. Through the combinations of inorganic and organic components in conjunction with appropriate processing methods, various types of primary and secondary bonding can be developed leading to materials with new properties for electrical, optical, structural, or related applications. [3] EXPERIMENTAL MATERIALS USED. DGEBA liquid epoxy resin (LY556) with epoxy equivalent around 170 and viscosity of 8000 to 12000 cp at 25 degree Celsius was used as received from Araldite India Pvt. Ltd.The silicon alkoxide, TEOS was supplied by Aldrich, USA. Dimethyldichlorosilane was used as silane coupling agent supplied by M/s Merck .Organo modified polysiloxane with molecular weight around 5000 was used as liquid rubber modifier as received from Resil chemicals Pvt Ltd. Triethylene tetramine (HY 951curing agent) was used as received from Araldite India Pvt.Ltd. PREPARATION OF LIQUID RUBBER MODIFIED EPOXY MATRIX. Amine containing polydimethylsiloxane was taken as liquid rubber modifier. Five phr of liquid rubber modifier was taken along with epoxy resin and the mixture was heated at 50 degree Celsius for 30 minutes with continuous stirring. Then the liquid rubber modified epoxy resin was allowed to cool in the room temperature. PREPARATION OF SILANE COUPLING AGENT TREATED EPOXY RESIN. Dichlorodimethylsilane was taken as silane coupling agent. The required amount of Dichlorodimethylsilane along with epoxy resin was heated at 60 degree Celsius with continuous stirring for 5 hours. The silane treated epoxy resin was left untouched for 4 to 5 hours. The same silane treatment procedure was carried out for Amine containing PDMS modified epoxy resin. PREPARATION OF EPOXY AND MODIFIED EPOXY HYBRID MATERIALS. The silica nano particles were prepared by hydrolysis of TEOS in ethanol medium. The reaction mixture (Water+TEOS+Ethanol) was stirred for 15 minutes in a glass beaker. Then the mixture was added to 50 ml epoxy resin and stirred continuously for 24 hours. The triethylene tetramine curing agent was added to in-situ silica precipitated epoxy resin at room temperature. Then the epoxy/silica hybrid material was cast between two polished mild steel plates and allowed to cure at room temperature for 24 hours. Then the cured material was post-cured at 150 degree Celsius for 3 hours. The above said procedure was repeated for Amine containing PDMS modified epoxy resin, silane treated epoxy resin, and silane treated Amine containing PDMS modified epoxy resin.
Page 1 and 2:
Design of experiments for optimizin
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Verification Experiments Confirmato
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Fig 3 Overlaid contour plots for te
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processing variables on the adhesio
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NR / CR TSC (%) 100 / 0 75 / 25 50
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the observed high values of its T-p
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Nondestructive testing of defects i
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visible impact damage (BVID). The c
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Fig 2. Photograph of the spliced ne
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Electrical studies on silver subsur
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temperatures exhibited by the 50 nm
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Figure 1: Variation of ln R with 1/
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Experimental Polyamide6 (PA6 with z
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Table 1: Sample code and compositio
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Blends of unsaturated polyester res
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in comparison to that of the base r
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Fig. 1 Tensile strength of rubber m
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characterization of PTT/m-LLDPE ble
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organoclay into the blend matrix re
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Figure: 5 - DSC cooling thermogram
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polypropylene exhibits β-chain sci
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ehavior. Here two possible effects
Page 45 and 46:
Complex modulus (KPa) Complex visco
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has been carried out using thermogr
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Weight (%) 80 40 0 Table 1. Sample
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Mechanical properties of natural ru
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due to adsorption on rubber particl
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Preparation and Characterization of
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2.7. Fabrication of curcumin elutin
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Table 2. Effect of curcumin content
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Biodegradable nanocomposites can be
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crystallization temperature of PBAT
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Biomimetic synthesis of nanohybrids
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3.3. Thermogravimetric analysis (TG
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Fig 2: 31 P-NMR Spectra of as-synth
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In this work we have examined the c
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7. George, K.M, Alex, R, Joseph, S
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Reinforcement studies - Effect of t
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Results and Discussion Immersion an
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Stress (MPa) 26 24 22 20 18 16 14 1
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Effect of plasticizer, filler and s
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Results and Discussion Properties o
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prepolymers having higher percentag
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Table2. Formulation for Peroxide cu
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Elongation at Break The elongation
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All-PP composites based on β and
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a T E'(T) = (1) E'(T ) ref The shif
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We tried the classical WLF equation
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Figure 2. Schematic of time-tempera
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Intercalated poly (methyl methacryl
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them. The nanocomposites prepared u
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Table 1: Mechanical Properties of P
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Abstract A Review on thermally stab
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processing of different commercial
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d(%Mass)/dT ( 0 d(%Mass)/dT ( C) 0
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composites has been reported to imp
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(a) (b) Figure 2: WAXD of a) PVC/mi
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Storage Modulus (M Pa) 3000 2500 20
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17. Peprnicek, T.; Duchet, J.; Kova
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constraint of several nanometers, t
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The FT-IR spectrum .ER-Epoxy resin,
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GLASS TRANSITION TEMPERATURE (Tg) V
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AFM image of Amine containing PDMS
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8. A.Al.Abrash, F.Al.Sagheer, A.A.m
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2. Experimental Details Polypropyle
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5. Acknowlegements We would like to
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Synthesis and characterization of p
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pristine polypropylene during cooli
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a Figure 2: Typical TEM micrographs
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potassium ditelluratoargentate (III
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found to be 80.51 and 77.31, respec
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14. G. Canche-Escamilla, J.I. Cauic
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2.2. Characterization of electrospu
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eported that tortuosity decreases w
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Abstract: Effect of nano TiO2 in co
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3. Results and Discussion : The wid
Page 154 and 155:
This is further evidenced from the
Page 156 and 157:
Transducer using Terfenol-D/epoxy c
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esults were compared. Measurements
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500 400 300 200 100 0 Magnetostrict
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Experimental Materials Natural crum
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It is known that for alkali and alk
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Polymer sample Table1. Ion uptake b
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Abstract Protein functionalized pol
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2.4 Analysis of Particle size of ul
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Table 1 Nano particle preparation o
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As the particle size is reduced, su
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Figure- 3 SEM micrograph of EFNP of
Page 178 and 179:
Excess PVA solution was drained off
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Figure 1. IR spectra of (I) PSF bas
Page 182 and 183:
Photodegradable polypropylene film
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were observed as a broad peak in th
Page 186 and 187:
Fig. 1. Carbonyl index variation of
Page 188 and 189:
Abstract Swelling behaviour of hydr
Page 190 and 191:
Swelling experiment Circular shaped
Page 192 and 193:
⎛ hθ D = π⎜ ⎜ ⎝ 4Q ∞
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21. Bajsic G, Rek V. J Appl Polym S
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log (C α - C t ) 1.0 0.9 0.8 0.7 0
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esistance [2]. For converting it to
Page 200 and 201:
References 1. Bob RJ, Underwater El
Page 202 and 203:
Figure-2 Insertion Loss behavior 0.
Page 204 and 205:
Development of epoxy based material
Page 206 and 207:
NOTATIONS USED A→E-55, AL-45.S.g-
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The Samples E, I, H and pure epoxy
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The combination B The combination I
Page 212 and 213:
Graft-copolymerization of cellulose
Page 214 and 215:
Once the free-radical species (A
Page 216 and 217:
References 1. Margaret I.P, Sau L.L
Page 218 and 219:
Design of experiments for optimizin
Page 220 and 221:
Verification Experiments Confirmato
Page 222 and 223:
Fig 3 Overlaid contour plots for te
Page 224 and 225:
processing variables on the adhesio
Page 226 and 227:
NR / CR TSC (%) 100 / 0 75 / 25 50
Page 228 and 229:
the observed high values of its T-p
Page 230 and 231:
Nondestructive testing of defects i
Page 232 and 233:
visible impact damage (BVID). The c
Page 234 and 235:
Fig 2. Photograph of the spliced ne
Page 236 and 237:
Electrical studies on silver subsur
Page 238 and 239:
temperatures exhibited by the 50 nm
Page 240 and 241:
Figure 1: Variation of ln R with 1/
Page 242 and 243:
Experimental Polyamide6 (PA6 with z
Page 244 and 245:
Table 1: Sample code and compositio
Page 246 and 247:
Blends of unsaturated polyester res
Page 248 and 249:
in comparison to that of the base r
Page 250 and 251:
Fig. 1 Tensile strength of rubber m
Page 252 and 253:
characterization of PTT/m-LLDPE ble
Page 254 and 255:
organoclay into the blend matrix re
Page 256 and 257:
Figure: 5 - DSC cooling thermogram
Page 258 and 259:
polypropylene exhibits β-chain sci
Page 260 and 261:
ehavior. Here two possible effects
Page 262 and 263:
Complex modulus (KPa) Complex visco
Page 264 and 265:
has been carried out using thermogr
Page 266 and 267:
Weight (%) 80 40 0 Table 1. Sample
Page 268 and 269:
Mechanical properties of natural ru
Page 270 and 271:
due to adsorption on rubber particl
Page 272 and 273:
Preparation and Characterization of
Page 274 and 275:
2.7. Fabrication of curcumin elutin
Page 276 and 277:
Table 2. Effect of curcumin content
Page 278 and 279:
Biodegradable nanocomposites can be
Page 280 and 281:
crystallization temperature of PBAT
Page 282 and 283:
Biomimetic synthesis of nanohybrids
Page 284 and 285:
3.3. Thermogravimetric analysis (TG
Page 286 and 287: Fig 2: 31 P-NMR Spectra of as-synth
Page 288 and 289: In this work we have examined the c
Page 290 and 291: 7. George, K.M, Alex, R, Joseph, S
Page 292 and 293: Reinforcement studies - Effect of t
Page 294 and 295: Results and Discussion Immersion an
Page 296 and 297: Stress (MPa) 26 24 22 20 18 16 14 1
Page 298 and 299: Effect of plasticizer, filler and s
Page 300: Results and Discussion Properties o
Page 303 and 304: prepolymers having higher percentag
Page 305 and 306: Table2. Formulation for Peroxide cu
Page 307 and 308: Elongation at Break The elongation
Page 309 and 310: All-PP composites based on β and
Page 311 and 312: a T E'(T) = (1) E'(T ) ref The shif
Page 313 and 314: We tried the classical WLF equation
Page 315 and 316: Figure 2. Schematic of time-tempera
Page 317 and 318: Intercalated poly (methyl methacryl
Page 319 and 320: them. The nanocomposites prepared u
Page 321 and 322: Table 1: Mechanical Properties of P
Page 323 and 324: Abstract A Review on thermally stab
Page 325 and 326: processing of different commercial
Page 327 and 328: d(%Mass)/dT ( 0 d(%Mass)/dT ( C) 0
Page 329 and 330: composites has been reported to imp
Page 331 and 332: (a) (b) Figure 2: WAXD of a) PVC/mi
Page 333 and 334: Storage Modulus (M Pa) 3000 2500 20
Page 335: 17. Peprnicek, T.; Duchet, J.; Kova
Page 339 and 340: The FT-IR spectrum .ER-Epoxy resin,
Page 341 and 342: GLASS TRANSITION TEMPERATURE (Tg) V
Page 343 and 344: AFM image of Amine containing PDMS
Page 345 and 346: 8. A.Al.Abrash, F.Al.Sagheer, A.A.m
Page 347 and 348: 2. Experimental Details Polypropyle
Page 349 and 350: 5. Acknowlegements We would like to
Page 351 and 352: Synthesis and characterization of p
Page 353 and 354: pristine polypropylene during cooli
Page 355 and 356: a Figure 2: Typical TEM micrographs
Page 357 and 358: potassium ditelluratoargentate (III
Page 359 and 360: found to be 80.51 and 77.31, respec
Page 361 and 362: 14. G. Canche-Escamilla, J.I. Cauic
Page 363 and 364: 2.2. Characterization of electrospu
Page 365 and 366: eported that tortuosity decreases w
Page 367 and 368: Abstract: Effect of nano TiO2 in co
Page 369 and 370: 3. Results and Discussion : The wid
Page 371 and 372: This is further evidenced from the
Page 373 and 374: Transducer using Terfenol-D/epoxy c
Page 375 and 376: esults were compared. Measurements
Page 377 and 378: 500 400 300 200 100 0 Magnetostrict
Page 379 and 380: Experimental Materials Natural crum
Page 381 and 382: It is known that for alkali and alk
Page 383 and 384: Polymer sample Table1. Ion uptake b
Page 385 and 386: Abstract Protein functionalized pol
Page 387 and 388:
2.4 Analysis of Particle size of ul
Page 389 and 390:
Table 1 Nano particle preparation o
Page 391 and 392:
As the particle size is reduced, su
Page 393 and 394:
Figure- 3 SEM micrograph of EFNP of
Page 395 and 396:
Excess PVA solution was drained off
Page 397 and 398:
Figure 1. IR spectra of (I) PSF bas
Page 399 and 400:
Photodegradable polypropylene film
Page 401 and 402:
were observed as a broad peak in th
Page 403 and 404:
Fig. 1. Carbonyl index variation of
Page 405 and 406:
Abstract Swelling behaviour of hydr
Page 407 and 408:
Swelling experiment Circular shaped
Page 409 and 410:
⎛ hθ D = π⎜ ⎜ ⎝ 4Q ∞
Page 411 and 412:
21. Bajsic G, Rek V. J Appl Polym S
Page 413 and 414:
log (C α - C t ) 1.0 0.9 0.8 0.7 0
Page 415 and 416:
esistance [2]. For converting it to
Page 417 and 418:
References 1. Bob RJ, Underwater El
Page 419 and 420:
Figure-2 Insertion Loss behavior 0.
Page 421 and 422:
Development of epoxy based material
Page 423 and 424:
NOTATIONS USED A→E-55, AL-45.S.g-
Page 425 and 426:
The Samples E, I, H and pure epoxy
Page 427 and 428:
The combination B The combination I
Page 429 and 430:
Graft-copolymerization of cellulose
Page 431 and 432:
Once the free-radical species (A
Page 433 and 434:
References 1. Margaret I.P, Sau L.L
Page 435 and 436:
Studies on processing of styrene bu
Page 437 and 438:
3 Results 4. Swelling index - Tolue
Page 439:
4. Swelling index The swelling indi
Page 442 and 443:
Effect of post drawing parameters o
Page 444 and 445:
Drawing the fiber at 100 0 C, which
Page 446 and 447:
Table 1: Experimental details of va
Page 448 and 449:
and the primary variables in the go
Page 450 and 451:
The equ (3.2) is linearized and we
Page 452 and 453:
Initial Deformed coordinates coordi
Page 454 and 455:
As 'C' channel structures is non-sy
Page 456 and 457:
Figure 3: Von-mises stress distribu
Page 458 and 459:
Synthesis, curing and characterizat
Page 460 and 461:
Results and Discussion: . Table 4.1
Page 462 and 463:
TGDDM/DDM SYSTEM: There are 2 trans
Page 464 and 465:
Table 4.6: DSC Results DSC thermo g
Page 466 and 467:
CONCLUSION: 1. Tetraglycidyl Diamin
Page 468 and 469:
Studies on processing of styrene bu
Page 470 and 471:
3 Results 4. Swelling index - Tolue
Page 472:
4. Swelling index The swelling indi
Page 475 and 476:
Effect of post drawing parameters o
Page 477 and 478:
Drawing the fiber at 100 0 C, which
Page 479 and 480:
Table 1: Experimental details of va
Page 481 and 482:
and the primary variables in the go
Page 483 and 484:
The equ (3.2) is linearized and we
Page 485 and 486:
Initial Deformed coordinates coordi
Page 487 and 488:
As 'C' channel structures is non-sy
Page 489 and 490:
Figure 3: Von-mises stress distribu
Page 491 and 492:
Synthesis, curing and characterizat
Page 493 and 494:
Results and Discussion: . Table 4.1
Page 495 and 496:
TGDDM/DDM SYSTEM: There are 2 trans
Page 497 and 498:
Table 4.6: DSC Results DSC thermo g
Page 499 and 500:
CONCLUSION: 1. Tetraglycidyl Diamin
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