Rheological properties of dental resin cements during polymerization

Jae-Rim Lee; Jai-Bong Lee; Jung-Suk Han; Sung-Hun Kim; In-Sung Yeo; Seung-Ryong Ha; Hee-Kyung Kim

doi:10.4047/jkap.2014.52.2.82

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Lee, Lee, Han, Kim, Yeo, Ha, and Kim: Rheological properties of dental resin cements during polymerization

ORIGINAL ARTICLE

J Korean Acad Prosthodont 2014;52(2):82-89.

Published online: 18 January 2014

DOI: https://doi.org/10.4047/jkap.2014.52.2.82

Rheological properties of dental resin cements during polymerization

Jae-Rim Lee¹, Jai-Bong Lee^1,^∗, Jung-Suk Han¹, Sung-Hun Kim¹, In-Sung Yeo¹, Seung-Ryong Ha², Hee-Kyung Kim³

^¹Department of Prosthodontics and Dental Research Institute, School of Dentistry, Seoul National University, Seoul, Republic of Korea

^²Department of Dentistry, Ajou University, School of Medicine, Suwon, Republic of Korea

^³Department of Prosthodontics, Veterans Health Service Medical Center Seoul, Republic of Korea

∗Corresponding Author: Jai-Bong Lee Department of Prosthodontics and Dental Research Institute, School of Dentistry, Seoul National University, 275-1, Yeongeon-dong, Jongno-gu, Seoul, 110-768, Republic of Korea +82 2 2072 2661: e-mail, swallow@snu.ac.kr

Received 10 March 201414 April 2014 Accepted 17 April 2014

This is an Open Access article distributed under the terms of the Creative Commons Attribution Non-Commercial License (http://creativecommons.org/licenses/by-nc/3.0/) which permits unrestricted non-commercial use, distribution, and reproduction in any medium, provided the original work is properly cited.

Abstract

Purpose

The purpose of this study was to observe the change of viscoelastic properties of dental resin cements during polymerization.

Materials and methods

Six commercially available resin cement materials (Clearfil SA luting, Panavia F 2.0, Zirconite, Variolink N, RelyX Unicem clicker, RelyX U200) were investigated in this study. A dynamic oscillation-time sweep test was performed with AR1500 stress controlled rheometer at 32℃. The changes in shear storage modulus (G'), shear loss modulus (G”), loss tangent (tan δ) and displacement were measured for twenty minutes and repeated three times for each material. The data were analyzed using one-way ANOVA and Tukey's post hoc test (α =0.05).

Results

After mixing, all materials demonstrated an increase in G' with time, reaching the plateau in the end. RelyX U200 demonstrated the highest G' value, while RelyX Unicem (clicker type) and Variolink N demonstrated the lowest G' value at the end of experimental time. Tan δ was maintained at some level and reached the zero at the starting point where G' began to increase. The tan δ and displacement of the tested materials showed similar pattern in the graph within change of time. The displacement of all 6 materials approached to zero within 6 minutes.

Conclusion

Compared to other resin cements used in this study, RelyX U200 maintained plastic property for a longer period of time. When it completed the curing process, RelyX U200 had the highest stiffness. It is convenient for clinicians to cement multiple units of dental prostheses simultaneously. (J Korean Acad Prosthodont 2014;52:82-9)

Keywords: Dental resin cement, Rheological properties, Film thickness, Viscoelasticity

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Fig. 1.

Dynamic oscillatory time sweep testing involves the application strain to a resin cement material and to record the resultant stress. The phase angle (δ) and the ratio of stress amplitude and strain amplitude allow the calculation of the shear storage modulus (G'), loss modulus (G''), loss tangent (tan δ) and other rheological variables.

Fig. 2.

The representative of shear storage modulus (G') of dental resin cements investigated. The increase of G' means the progression of the cross-linking and entanglements of polymer chains. It means that the material shows the onset of elasticity or loss of fluidity. Initial setting time is defined as amount of time until beginning of the development of elasticity, such as increase of the value of G' or decrease of the value of tan δ .

Fig. 3.

The representative of shear loss modulus (G") of dental resin cements investigated.

Fig. 4.

The representative of loss tangent (tan δ) of dental resin cements investigated. The value of tan δ depends on the ratio of G'' to G'. It represents loss of plasticity and corresponds with tendency of displacement curve.

Fig. 5.

The representative of displacement of dental resin cements investigated.

Table 1.

Dental resin cement materials included in this study

Material	Manufacturer	Bat. No.	Composition	Filler contents	Mean particle size (㎛)
RelyX U200	3M ESPE (MN, USA)	487972	Bi-functional (meth)acrylate	43 wt%	12.5
(Automix)
RelyX Unicem	3M ESPE (MN, USA)	474045	Bi-functional (meth)acrylate	70 wt%	12.5
(Clicker type)
Clearfil SA Luting	Kuraray	0374AA	Paste A : Bis-GMA, TEGDMA, 10-MDP,	44 vol%	2.5
(Clicker type)	(Noritake Dental Inc.,		Hydrophobic aromatic dimethacrylate,	5 wt%
	Okayama, Japan)		Silanated barium glass filler, Silanated colloidal sillica,
			di-Camphorquinone, Initiators, Benzoyl peroxide
			Paste B : Bis-GMA, Hydrophobic aromatic dimethacrylate,
			Hydrophobic aliphatix dimethacrylate, Silanated barium glass filler,
			Silanated colloidal sillica, Accelerators, Pigments
Panavia F 2.0	Kuraray (Medical Inc.,	0558AA	A paste: 10-MDP, Hydrophobic aromatic dimethacrylate,	59 vol%	0.04 - 19
	Osaka, Japan)	0104AC	Hydrophobic aliphatic dimethacrylate,
			Hydrophilic aliphatic dimethacrylate, Silanated silica filler,
			Silanated colloidal silica, di-Camphorquinone, catalyst, Initiator
			B paste: Hydrophobic aromatic dimethacrylate,
			Hydrophobic aliphatic dimethacrylate, Silanated barium glass filler,
			Surface treated sodium fluoride, Catalyst, Accelerators, Pigments
Zirconite	BJM LAB (Israel)	4194HBARCZKR	Bis-GMA, UDMA Oligomer, TEGDMA, 4-META,	-	-
(Automix)			Methacrylated phosphoric acid esters,
			[3-(Methacryloyloxy)propyl] trimethoxysilane, photoinitiator,
			Co-initiator, Benzoyl peroxide, Barium aluminoborosilicate glass,
			fumed silica
Variolink N	Ivoclar vivadent	P72407 (Base)	Bis-GMA, UDMA, TEGDMA,	44 vol%	0.7
	(Schaan, Liechtenstein)	68646 (Catalyst)	Inorganic filler (barium glass, ytterbium trifluoride,	71 wt%	(0.04 - 3.0)
			Ba-Al-fluorosilicate glass, pheroid mixed oxide, Initiator,
			Stabilizer, Pigment

Table 2.

The storage moduli (G') and loss tangent (tan δ) at different elapsed times, setting times for the dental resin cement materials during polymerization at 32℃

Material	t = 1 min		t = 5 min		t = 20 min
Material	G' (Pa)	tan δ	G' (Pa)	tan δ	G' (Pa)	tan δ
RelyX U200 (Automix)	0.41	50.04	5.07E + 06	0.10	7.33E + 06	0.02
RelyX Unicem (clicker type)	2.81	18.46	3.41E + 06	0.06	3.74E + 06	0.02
Clearfil SA Luting	2.55	21.66	1.71E + 06	0.16	3.88E + 06	0.01
Panavia F 2.0	3.46	16.14	1.14E + 05	0.24	4.65E + 06	0.03
Zirconite	0.30	81.45	4.59E + 06	0.05	5.04E + 06	0.02
Variolink N	57.91	3.83	5.75E + 03	0.46	3.67E + 06	0.01

Table 3.

The initial setting time, setting time and G' at the plateau different elapsed times, setting times for the dental resin cement materials during polymerization at 32℃

Material	Initial setting time (s)	Setting time at T90 (s)	Shear storage modulus (G') (MPa)
RelyX U200	197.50 (13.42)^c	538.13 (24.95)^g	7.25 (0.22)ⁱ
RelyX Unicem	150.16 (5.04)^d	352.70 (22.61)^h	3.73 (0.11)^l
Clearfil SA Luting	156.73 (8.92)^d	613.20 (5.45)^f	3.84 (0.10)^l
Zirconite	168.22 (76.82)^d	356.46 (9.95)^h	5.02 (0.07)^j
Panavia F 2.0	303.37 (5.23)^b	635.6 (14.57)^f	4.66 (0.10)^k
Variolink N	338.80 (11.20)^a	801.98 (24.86)^e	3.62 (0.09)^l

∗ Numbers in parentheses are standard deviations.

The same superscript letters in the same column indicate no significant differences respectively (Tukey's post hoc test: P>.05).

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