318:
131:
66:
155:
828:) and has the capability of monitoring the resin cure throughout the entire cycle, from the liquid to the rubber to the solid state. It is capable of monitoring phase separation in complex resin blends curing also within a fibrous perform. The same attributes belong to the more recent development of the dielectric technique, namely microdielectrometry.
831:
Several versions of dielectric sensors are available commercially. The most suitable format for use in cure monitoring applications are the flat interdigital capacitive structures bearing a sensing grid on their surface. Depending on their design (specifically those on durable substrates) they have
358:
As shown in Figure 4, after an "induction time", G' and G" start to increase, with an abrupt change in slope. At a certain point they cross each other; afterwards, the rates of G' and G" decrease, and the moduli tend to a plateau. When they reach the plateau the reaction is concluded.
679:
1166:
Harkous, Ali; Colomines, Gaël; Leroy, Eric; Mousseau, Pierre; Deterre, Rémi (April 2016). "The kinetic behavior of Liquid
Silicone Rubber: A comparison between thermal and rheological approaches based on gel point determination".
497:
211:
that largely comprise them. When paint is described as "drying" it is in fact hardening by crosslinking. Oxygen atoms serve as the crosslinks, analogous to the role played by sulfur in the vulcanization of rubber.
501:
The degree of curing starts from zero (at the beginning of the reaction) and grows until one (the end of the reaction). The slope of the curve changes with time and has his maximum about at half of the reaction.
227:
In many cases, the resin is provided as a solution or mixture with a thermally-activated catalyst, which induces crosslinking but only upon heating. For example, some acrylate-based resins are formulated with
362:
When the system is liquid, the storage modulus is very low: the system behaves like a liquid. Then the reaction continues and the system starts to react more like a solid: the storage modulus increases.
809:
Also in this case the degree of curing goes from zero (no bonds created) to one (no more reactions occur) with a slope that changes in time and has its maximum about at half of the reaction.
122:
The curing methodology depends on the resin and the application. Particular attention is paid to the shrinkage induced by the curing. Usually small values of shrinkage (2–3%) are desirable.
69:
Figure 1: Structure of a cured epoxy glue. The triamine hardener is shown in red, the resin in black. The resin's epoxide groups have reacted with the hardener. The material is highly
558:
1273:
I.Partridge and G.Maistros, 'Dielectric Cure
Monitoring for Process Control', Chapter 17, Vol. 5, Encyclopaedia of Composite Materials (2001), Elsevier Science, London, page 413
1055:
980:
750:
551:
384:
804:
777:
721:
701:
1018:
Chambon, Francois; Winter, H. Henning (November 1987). "Linear
Viscoelasticity at the Gel Point of a Crosslinking PDMS with Imbalanced Stoichiometry".
849:
77:
During the curing process, single monomers and oligomers, mixed with or without a curing agent, react to form a tridimensional polymeric network.
325:
A simple way to monitor the change in viscosity, and thus, the extent of the reaction, in a curing process is to measure the variation of the
1264:
1243:
1147:
1097:
119:. An intermediate case involves a mixture of resin and additives that requires external stimulus (light, heat, radiation) to induce curing.
518:
created, higher is the heat released in the reaction. At the end of the reaction, no more heat will be released. To measure the heat flow
391:
134:
Figure 2: General representation of the chemical structure of vulcanized natural rubber showing the crosslinking of two polymer chains (
1072:
997:
88:
increases in time with the extent of the reaction until the network size is equal to the size of the system. The system has lost its
519:
53:, the term "curing" can be used for all the processes where a solid product is obtained from a liquid solution, such as with PVC
832:
some reusability, while flexible substrate sensors can be used also in the bulk of the resin systems as embedded sensors.
317:
232:. Upon heating the mixture, the peroxide converts to a free radical, which adds to an acrylate, initiating crosslinking.
81:
1294:
349:
345:
341:
1289:
871:
196:. The degree of crosslinking determines the rigidity and durability, as well as other properties of the material.
674:{\displaystyle \alpha ={\frac {Q}{Q_{T}}}={\frac {\int _{0}^{s}{\dot {Q}}\,dt}{\int _{0}^{s_{f}}{\dot {Q}}\,dt}}}
263:
the system is relatively mobile, after it the mobility is very limited, the micro-structure of the resin and the
1276:
P.Ciriscioli and G.Springer, 'Smart
Autoclave cure in Composites', (1991), Technomic Publishing, Lancaster, PA.
890:
cure monitoring methods are based on the relationships between changes in the characteristics of propagating
166:. In the second step, the hydroperoxide combines with another unsaturated side chain to generate a crosslink.
1203:
Hong, In-Kwon; Lee, Sangmook (January 2013). "Cure kinetics and modeling the reaction of silicone rubber".
514:, the crosslinking rate can be related to the heat released during the process. Higher is the number of
290:
Cure monitoring is, for example, an essential component for the control of the manufacturing process of
279:
158:
Figure 3: Simplified chemical reactions associated with curing of a drying oil. In the first step, the
50:
111:: curing "might or might not require mixing with a chemical curing agent". Thus, two broad classes are
130:
1027:
185:
355:
can be measured. The variation of G' and G" in time can indicate the extent of the curing reaction.
875:
511:
291:
38:
853:
267:
is fixed and severe diffusion limitations to further cure are created. Thus, in order to achieve
264:
229:
726:
224:, curing entails the formation of silicate crosslinks. The process is not induced by additives.
321:
Figure 4: Evolution in time of storage modulus G' and loss modulus G" during a curing reaction.
184:, the curing is also induced by the addition of a crosslinker. The resulting process is called
107:
Curing can be induced by heat, radiation, electron beams, or chemical additives. To quote from
100:
start to coexist with the macroscopic network until they react with the network creating other
1260:
1239:
1233:
1143:
1093:
1068:
993:
825:
817:
Conventional dielectrometry is carried out typically in a parallel plate configuration of the
34:
1254:
536:
369:
104:. The crosslink density increases until the system reaches the end of the chemical reaction.
1212:
1176:
1117:
1060:
1035:
985:
955:
860:
268:
200:
85:
782:
755:
1180:
333:
326:
1031:
706:
686:
1283:
919:
906:
526:
515:
204:
193:
163:
65:
864:
845:
1114:
Patterning
Dewetting in Thin Polymer Films by Spatially Directed Photocrosslinking
989:
947:
1229:
840:
The curing process can be monitored by measuring changes in various parameters:
271:
in the resin, it is usually necessary to increase the process temperature after
1216:
1121:
924:
891:
887:
818:
309:
Cure monitoring relies on monitoring various physical or chemical properties.
208:
189:
89:
46:
1064:
960:
898:
ultrasonic time of flight, both in through-transmission and pulse-echo modes;
49:
of polymer chains. Even if it is strongly associated with the production of
530:
337:
303:
244:
240:
236:
174:
101:
93:
70:
54:
17:
272:
260:
252:
248:
221:
97:
154:
1112:
Gregory T. Carroll, Nicholas J. Turro and
Jeffrey T. Koberstein (2010)
247:
interconnect. This process continues until a tridimensional network of
42:
894:
and the real-time mechanical properties of a component, by measuring:
173:
are typically cured by the use of additives, often called hardeners.
1039:
821:
295:
181:
147:
492:{\displaystyle \alpha ={\frac {G'(t)-G'_{min}}{G'_{max}-G'_{min}}}}
902:
316:
299:
256:
235:
Some organic resins are cured with heat. As heat is applied, the
170:
159:
153:
129:
108:
64:
306:
is the most important property that changes during the process.
1116:
Journal of
Colloid and Interface Science, Vol. 351, pp 556-560
177:
are often used. The amine groups ring-open the epoxide rings.
73:
and contains many OH groups, which confer adhesive properties.
844:
the concentration of specific reactive resin species using
533:
releases the same amount of energy, the degree of curing,
27:
Chemical process by which polymeric materials are hardened
1053:
Ulrich Poth (2002). "Drying Oils and
Related Products".
978:
Pham, Ha Q.; Marks, Maurice J. (2012). "Epoxy Resins".
785:
758:
729:
709:
689:
561:
539:
394:
372:
1140:
Rheology: principles, measurements, and applications
510:If the reactions occurring during crosslinking are
798:
771:
744:
715:
695:
673:
545:
491:
378:
84:with various architectures are formed, and their
112:
1205:Journal of Industrial and Engineering Chemistry
207:that catalyze cross-linking of the unsaturated
41:that produces the toughening or hardening of a
1056:Ullmann's Encyclopedia of Industrial Chemistry
981:Ullmann's Encyclopedia of Industrial Chemistry
901:natural frequency using impact excitation and
116:
8:
243:, whereupon it increases as the constituent
1235:Materials science of polymers for engineers
115:(also called curing agents, hardeners) and
703:is the heat released up to a certain time
1088:James E. Mark; Burak Erman, eds. (2005).
973:
971:
959:
790:
784:
763:
757:
731:
730:
728:
708:
688:
661:
650:
649:
641:
636:
631:
618:
607:
606:
600:
595:
588:
577:
568:
560:
538:
471:
449:
428:
401:
393:
371:
251:chains is created – this stage is termed
188:. Sulfur breaks down to form polysulfide
779:is the total amount of heat released in
1161:
1159:
942:
940:
936:
239:of the resin drops before the onset of
80:In the very first part of the reaction
874:(mechanical property) with the use of
752:is the instantaneous rate of heat and
259:this marks an important stage: before
199:Paints and varnishes commonly contain
1198:
1196:
1194:
1192:
1190:
1181:10.1016/j.reactfunctpolym.2016.01.020
1133:
1131:
1129:
1013:
1011:
1009:
7:
1259:. Vincentz Network. pp. 11–16.
298:, at the end of the process will be
255:. In terms of processability of the
113:curing induced by chemical additives
1238:. Hanser Verlag. pp. 334–335.
192:(bridges) between sections of the
117:curing in the absence of additives
33:is a chemical process employed in
25:
520:differential scanning calorimetry
282:, the process is called UV cure.
162:undergoes autoxidation to give a
96:tends to infinite. The remaining
1169:Reactive and Functional Polymers
1138:Macosko, Christopher W. (1994).
1090:Science and technology of rubber
867:of the resin (optical property);
278:When catalysts are activated by
806:, when the reaction finishes.
418:
412:
1:
990:10.1002/14356007.a09_547.pub2
553:, can be defined as follows:
336:of a system during curing, a
386:, can be defined as follow:
342:dynamic mechanical analysis
126:Curing induced by additives
1311:
1253:Glöckner, Patrick (2009).
1217:10.1016/j.jiec.2012.05.006
1122:10.1016/j.jcis.2010.07.070
745:{\displaystyle {\dot {Q}}}
294:. The material, initially
876:Fiber Bragg grating (FBG)
1232:; Menges, Georg (2003).
1065:10.1002/14356007.a09_055
961:10.1351/goldbook.CT07137
813:Dielectrometric analysis
216:Curing without additives
1059:. Weinheim: Wiley-VCH.
984:. Weinheim: Wiley-VCH.
546:{\displaystyle \alpha }
379:{\displaystyle \alpha }
836:Spectroscopic analysis
800:
773:
746:
717:
697:
675:
547:
493:
380:
366:The degree of curing,
322:
167:
151:
74:
51:thermosetting polymers
909:velocity measurement.
846:spectroscopic methods
801:
799:{\displaystyle s_{f}}
774:
772:{\displaystyle Q_{T}}
747:
718:
698:
676:
548:
494:
381:
320:
280:ultraviolet radiation
157:
133:
82:branches of molecules
68:
1142:. VCH. p. 568.
783:
756:
727:
707:
687:
559:
537:
392:
370:
346:storage modulus (G')
313:Rheological analysis
186:sulfur vulcanization
1032:1987JRheo..31..683C
1020:Journal of Rheology
883:Ultrasonic analysis
870:the internal resin
648:
605:
525:Assuming that each
485:
463:
442:
292:composite materials
150:(n = 0, 1, 2, 3 …).
39:process engineering
1295:Chemical processes
796:
769:
742:
713:
693:
671:
627:
591:
543:
529:formed during the
489:
467:
445:
424:
376:
340:can be used. With
323:
286:Monitoring methods
265:composite material
230:dibenzoyl peroxide
168:
152:
75:
1290:Polymer chemistry
1266:978-3-86630-907-4
1245:978-1-56990-348-3
1149:978-0-471-18575-8
1099:978-0-12-464786-2
905:-induced surface
826:capacitance probe
739:
716:{\displaystyle s}
696:{\displaystyle Q}
669:
658:
615:
583:
487:
201:oil drying agents
35:polymer chemistry
16:(Redirected from
1302:
1270:
1256:Radiation Curing
1249:
1221:
1220:
1200:
1185:
1184:
1163:
1154:
1153:
1135:
1124:
1110:
1104:
1103:
1085:
1079:
1078:
1050:
1044:
1043:
1040:10.1122/1.549955
1015:
1004:
1003:
975:
966:
965:
963:
944:
861:refractive index
805:
803:
802:
797:
795:
794:
778:
776:
775:
770:
768:
767:
751:
749:
748:
743:
741:
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732:
722:
720:
719:
714:
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700:
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680:
678:
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672:
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660:
659:
651:
647:
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645:
635:
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617:
616:
608:
604:
599:
589:
584:
582:
581:
569:
552:
550:
549:
544:
506:Thermal analysis
498:
496:
495:
490:
488:
486:
481:
459:
443:
438:
411:
402:
385:
383:
382:
377:
145:
139:
86:molecular weight
21:
1310:
1309:
1305:
1304:
1303:
1301:
1300:
1299:
1280:
1279:
1267:
1252:
1246:
1230:Osswald, Tim A.
1228:
1225:
1224:
1202:
1201:
1188:
1165:
1164:
1157:
1150:
1137:
1136:
1127:
1111:
1107:
1100:
1092:. p. 768.
1087:
1086:
1082:
1075:
1052:
1051:
1047:
1017:
1016:
1007:
1000:
977:
976:
969:
946:
945:
938:
933:
916:
885:
838:
815:
786:
781:
780:
759:
754:
753:
725:
724:
705:
704:
685:
684:
637:
626:
590:
573:
557:
556:
535:
534:
508:
444:
404:
403:
390:
389:
368:
367:
350:loss modulus (G
334:elastic modulus
332:To measure the
327:elastic modulus
315:
288:
220:In the case of
218:
141:
135:
128:
63:
28:
23:
22:
15:
12:
11:
5:
1308:
1306:
1298:
1297:
1292:
1282:
1281:
1278:
1277:
1274:
1271:
1265:
1250:
1244:
1223:
1222:
1186:
1155:
1148:
1125:
1105:
1098:
1080:
1074:978-3527306732
1073:
1045:
1026:(8): 683–697.
1005:
999:978-3527306732
998:
967:
952:IUPAC Goldbook
935:
934:
932:
929:
928:
927:
922:
915:
912:
911:
910:
899:
884:
881:
880:
879:
868:
857:
837:
834:
814:
811:
793:
789:
766:
762:
738:
735:
712:
692:
667:
664:
657:
654:
644:
640:
634:
630:
624:
621:
614:
611:
603:
598:
594:
587:
580:
576:
572:
567:
564:
542:
507:
504:
484:
480:
477:
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462:
458:
455:
452:
448:
441:
437:
434:
431:
427:
423:
420:
417:
414:
410:
407:
400:
397:
375:
314:
311:
287:
284:
217:
214:
205:metallic soaps
194:polymer chains
127:
124:
62:
61:Curing process
59:
26:
24:
14:
13:
10:
9:
6:
4:
3:
2:
1307:
1296:
1293:
1291:
1288:
1287:
1285:
1275:
1272:
1268:
1262:
1258:
1257:
1251:
1247:
1241:
1237:
1236:
1231:
1227:
1226:
1218:
1214:
1210:
1206:
1199:
1197:
1195:
1193:
1191:
1187:
1182:
1178:
1174:
1170:
1162:
1160:
1156:
1151:
1145:
1141:
1134:
1132:
1130:
1126:
1123:
1119:
1115:
1109:
1106:
1101:
1095:
1091:
1084:
1081:
1076:
1070:
1066:
1062:
1058:
1057:
1049:
1046:
1041:
1037:
1033:
1029:
1025:
1021:
1014:
1012:
1010:
1006:
1001:
995:
991:
987:
983:
982:
974:
972:
968:
962:
957:
953:
949:
943:
941:
937:
930:
926:
923:
921:
920:Vulcanization
918:
917:
913:
908:
907:acoustic wave
904:
900:
897:
896:
895:
893:
889:
882:
877:
873:
869:
866:
862:
858:
855:
851:
847:
843:
842:
841:
835:
833:
829:
827:
823:
820:
812:
810:
807:
791:
787:
764:
760:
736:
733:
710:
690:
681:
665:
662:
655:
652:
642:
638:
632:
628:
622:
619:
612:
609:
601:
596:
592:
585:
578:
574:
570:
565:
562:
554:
540:
532:
528:
523:
522:can be used.
521:
517:
513:
505:
503:
499:
482:
478:
475:
472:
468:
464:
460:
456:
453:
450:
446:
439:
435:
432:
429:
425:
421:
415:
408:
405:
398:
395:
387:
373:
364:
360:
356:
354:
353:
347:
343:
339:
335:
330:
328:
319:
312:
310:
307:
305:
301:
297:
293:
285:
283:
281:
276:
274:
270:
269:vitrification
266:
262:
258:
254:
250:
246:
242:
238:
233:
231:
225:
223:
215:
213:
210:
206:
202:
197:
195:
191:
187:
183:
178:
176:
172:
165:
164:hydroperoxide
161:
156:
149:
144:
138:
132:
125:
123:
120:
118:
114:
110:
105:
103:
99:
95:
91:
87:
83:
78:
72:
67:
60:
58:
56:
52:
48:
47:cross-linking
44:
40:
36:
32:
19:
1255:
1234:
1211:(1): 42–47.
1208:
1204:
1172:
1168:
1139:
1113:
1108:
1089:
1083:
1054:
1048:
1023:
1019:
979:
951:
886:
865:fluorescence
839:
830:
816:
808:
682:
555:
531:crosslinking
524:
509:
500:
388:
365:
361:
357:
351:
331:
324:
308:
289:
277:
241:crosslinking
234:
226:
219:
198:
179:
171:Epoxy resins
169:
142:
136:
121:
106:
79:
76:
45:material by
30:
29:
18:Curing agent
209:drying oils
190:cross-links
71:crosslinked
1284:Categories
931:References
925:Cross-link
892:ultrasound
888:Ultrasonic
819:dielectric
512:exothermic
203:, usually
175:Polyamines
102:crosslinks
90:solubility
55:plastisols
1175:: 20–27.
737:˙
656:˙
629:∫
613:˙
593:∫
563:α
541:α
465:−
422:−
396:α
374:α
338:rheometer
304:viscosity
245:oligomers
237:viscosity
98:molecules
94:viscosity
954:. 2014.
948:"curing"
914:See also
878:sensors.
848:such as
483:′
461:′
440:′
409:′
348:and the
273:gelation
261:gelation
253:gelation
249:oligomer
222:concrete
92:and its
1028:Bibcode
146:) with
43:polymer
1263:
1242:
1146:
1096:
1071:
996:
872:strain
852:&
822:sensor
683:where
344:, the
296:liquid
182:rubber
148:sulfur
31:Curing
903:laser
854:Raman
516:bonds
300:solid
257:resin
160:diene
143:green
109:IUPAC
1261:ISBN
1240:ISBN
1144:ISBN
1094:ISBN
1069:ISBN
994:ISBN
859:the
850:FTIR
527:bond
140:and
137:blue
37:and
1213:doi
1177:doi
1173:101
1118:doi
1061:doi
1036:doi
986:doi
956:doi
863:or
180:In
1286::
1209:19
1207:.
1189:^
1171:.
1158:^
1128:^
1067:.
1034:.
1024:31
1022:.
1008:^
992:.
970:^
950:.
939:^
723:,
329:.
302::
275:.
57:.
1269:.
1248:.
1219:.
1215::
1183:.
1179::
1152:.
1120::
1102:.
1077:.
1063::
1042:.
1038::
1030::
1002:.
988::
964:.
958::
856:;
824:(
792:f
788:s
765:T
761:Q
734:Q
711:s
691:Q
666:t
663:d
653:Q
643:f
639:s
633:0
623:t
620:d
610:Q
602:s
597:0
586:=
579:T
575:Q
571:Q
566:=
479:n
476:i
473:m
469:G
457:x
454:a
451:m
447:G
436:n
433:i
430:m
426:G
419:)
416:t
413:(
406:G
399:=
352:)
20:)
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