Journal List > J Korean Acad Conserv Dent > v.29(6) > 1056140

Lee, Lee, Cho, Lee, and Um: RHEOLOGICAL PROPERTIES OF RESIN COMPOSITES ACCORDING TO THE CHANGE OF MONOMER AND FILLER COMPOSITIONS

ABSTRACT

Objectives.

The aim of this study was to investigate the effect of monomer and filler compositions on the rheological properties related to the handling characteristics of resin composites.

Methods.

Resin matrices that Bis-GMA as base monomer was blended with TEGDMA as diluent at various ratio were mixed with the Barium glass (0.7 um and 1.0 um), 0.04 um fumed silica and 0.5 um round silica. All used fillers were silane treated. In order to vary the viscosity of experimental composites, the type and content of incorporated fillers were changed.
Using a rheometer, a steady shear test and a dynamic oscillatory shear test were used to evaluate the viscosity (η) of resin matrix, and the storage shear modulus (G′), the loss shear modulus (G″), the loss tangent (tanδ) and the complex viscosity (η *) of the composites as a function of frequency ω = 0.1-100 rad/s. To investigate the effect of temperature on the viscosity of composites, a temperature sweep test was also undertaken.

Results.

Resin matrices were Newtonian fluid regardless of diluent concentration and all experimental composites exhibited pseudoplastic behavior with increasing shear rate. The viscosity of composites was exponentially increased with increasing filler volume%. In the same filler volume, the smaller the fillers were used, the higher the viscosities were. The effect of filler size on the viscosity was increased with increasing filler content. Increasing filler content reduced tanδby increasing the G′further than the G″ . The viscosity of composites was decreased exponentially with increasing temperature.

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Figure 1.
Relationship between shear storage modulus (G′), shear loss modulus (G″), complex shear modulus (G*) and loss tangent (tanδ) in a complex plane.
jkacd-29-520f1.tif
Figure 2-a.
Viscosity of monomer blends of varying diluent’s concentration as a function of shear rates at 25℃.
jkacd-29-520f2a.tif
Figure 2-b.
Steady shear viscosity, η, and dynamic complex viscosity, η*, of Bis-GMA only and Bis-GMA 6 : TEGDMA 4 blend at 25℃ and 35℃.
jkacd-29-520f2b.tif
Figure 2-c.
Viscosity as a function of diluent fraction at temperature 25℃ and 35℃.
jkacd-29-520f2c.tif
Figure 3-a.
Complex viscosity of experimental composites of varying filler contents (weight%) as a function of frequency.
jkacd-29-520f3a.tif
Figure 3-b.
The effect of filler size and filler volume% on the complex viscosity of experimental composites at ω= 10 rad/s.
jkacd-29-520f3b.tif
Figure 3-c.
Exponential regression curve, y = aebx, can be fitted on the complex viscosity of experimental composite with 0.5 um Silica as a function of filler volume fraction.
jkacd-29-520f3c.tif
Figure 4-a.
The change of storage modulus G′and loss modulus G″with increasing filler content in 0.7um Ba glass.
jkacd-29-520f4a.tif
Figure 4-b.
Loss tangent (Tanδ) of experimental composites as a function of filler volume %.
jkacd-29-520f4b.tif
Figure 5.
Complex viscosity of experimental composites is exponentially decreased with increasing temperature.
jkacd-29-520f5.tif
Figure 6.
Complex viscosity of experimental and commercial composites as a function of frequency.
jkacd-29-520f6.tif
Figure 7-a.
Phasor representations of complex modulus G* and phase angle, δ, G*e= G*∠δ, of experimental and commercial composites at ω= 10 rad/s in a polar coordinate system.
jkacd-29-520f7a.tif
Figure 7-b.
Locus of frequency domain phasor plots, G*(ω )e=G*(ω )∠δ, of composites at ω= 0.1 - 100 rad/s in a complex plane.
jkacd-29-520f7b.tif
Table 1.
Monomers and inorganic fillers used to make experimental composites and commercial composites.
Monomers
  Bis-GMA 2,2-bis-[4-(methacryloxy-2-hydroxy-propoxy)-phenyl]-propane
Manufacturer; Aldrichi, Germany
  TEGDMA Triethylene glycol dimethacrylate
Manufacturer; Aldrichi, Germany
Inorganic fillers
  Filler Type Abbreviation Manufacturer
  1) 0.7 um barium glass irregular 0.7 um Ba Schott, Germany
  2) 1.0 um barium glass irregular 1.0 um Ba Schott, Germany
  3) 40 ㎚ fumed silica (Aerosil OX-50) round 0.04 um Silica Degussa, Germany
  4) 0.5 um silica round 0.5 um Silica Youthtech, Korea
Commercial Composite
  Z100 3M, USA
  Charisma Kulzer, Germany
  Clearfil Kuraray, Japan
  DenFil Vericom, Koreea
Table 2.
The experimental composites were made with various types, size and weight% (the unit of the numbers in the parenthesis are volume%) of fillers added to resin matrix (Bis-GMA 6 : TEGDMA 4).
(1) 0.7 um Ba
50 (30.3), 60 (39.5), 70 (50.4), 75 (56.7) wt%
(2) 1.0 um Ba
60 (39.5), 75 (56.7) wt%
(3) 0.04 um Silica
30 (19.7), 40 (27.6), 50 (36.4), 55.9 (42.1) wt%
(4) 0.5 um Silica
30 (19.3), 35 (23.1), 40 (27.1), 45 (31.3) wt%
(5) 0.7 um Ba 70 wt% + 0.04 um Silica 5 wt% - hybrid composite (57.2 vol%)
(6) 0.7 um Ba 65 wt% + 0.04um Silica 10 wt% - hybrid composite (57.7 vol%)
Table 3.
The shear viscosity of monomer blends at 25 ℃ and 35℃.
Monomer blends Shear viscosity (Pa.s)
Bis-GMA vs. TEGDMA 25 ℃ 35 ℃
Bis-GMA only 369 52.6
8 : 2 5.04 1.46
7 : 3 1.280 0.476
6 : 4 0.429 0.203
5 : 5 0.144 0.085
4 : 6 0.066 0.021
3 : 7 0.035 0.0213
2 : 8 0.022 0.014
TEGDMA only 0.0077 0.0068
Table 4.
The phasor presentation of complex modulus G* and phase angle δ, G*(ω )e=G*(ω )∠δ , and the complex viscosity η* of experimental and commercial composites at 25℃.
Composites G* (Pa) ∠ δ(°) η* (Pa.s)
ω= 0.1 rad/s ω= 1 rad/s ω= 10 rad/s ω= 10 rad/s
0.7 um Ba
  50 wt% 17.7 ∠ 55. 3 43.6 ∠ 58. 1 129.3 ∠ 72.3 12.9
  60 wt% 55.3 ∠ 43. 9 81.2 ∠ 53. 3 205.9∠ 69.5 20.6
  70 wt% 48.6 ∠ 39. 1 111.8 ∠ 48. 2 311.2 ∠ 67.1 31.1
  75 wt% 137.5 ∠ 40. 8 280.2 ∠ 44. 1 610.5 ∠ 61.1 61.1
1 um Ba
  60 wt% 5.3 ∠ 50. 2 23.3 ∠ 60. 9 108.4 ∠ 74.9 10.8
  75 wt% 46.7 ∠ 42. 4 117.1 ∠ 50. 7 348.1 ∠ 69.0 34.8
0.04 um Silica
  30 wt% 235.0 ∠ 53. 5 95.9 ∠ 62. 9 235.0 ∠ 71.7 23.5
  40 wt% 240.1 ∠ 61.34 768.2 ∠ 57. 9 1274.0 ∠ 65.1 127.4
  50 wt% 1792.8 ∠ 57. 4 2982.2 ∠ 48. 6 4179.0 ∠ 51.3 417.9
  55.9 wt% 6202.9 ∠ 42. 8 4710.4 ∠ 41. 8 6453.0 ∠ 43.7 645.3
0.5 um Silica
  30 wt% 4.0 ∠ 71. 0 14.4 ∠ 79. 0 65.4 ∠ 83.2 6.5
  35 wt% 9.0 ∠ 68. 9 23.5 ∠ 75. 6 91.9 ∠ 82.3 9.2
  40 wt% 18.9 ∠ 66. 3 42.9 ∠ 71. 0 120.9 ∠ 81.5 12.1
  45 wt% 39.0 ∠ 63. 1 74.8 ∠ 65. 2 169.8 ∠ 77.7 17.0
0.7 um Ba 70 wt% + 0.04 um Silica 5 wt%
370.3 ∠ 40. 5 690.6 ∠ 39. 0 1299.5 ∠ 49.3 129.9
0.7 um Ba 65 wt% + 0.04 um Silica 10 wt%
1334.4 ∠ 35. 2 1683.8 ∠ 33.32 2600.0 ∠ 41.2 260.0
Z100 288.9 ∠ 32. 2 937.4 ∠ 30. 0 2080.0 ∠ 40.1 208.0
Charisma 164.4 ∠ 52. 3 475.1 ∠ 54. 5 1449.3 ∠ 64.9 144.9
Clearfil 1006.9 ∠ 61. 9 1575.7 ∠ 62. 3 3881.7 ∠ 73.5 388.2
DenFil 1881.0 ∠ 34. 0 3585.5 ∠ 32. 3 6525.7 ∠ 37.1 652.6
Table 5.
Regression analysis of the complex viscosity of the experimental composites as a function of filler volume fraction. The exponential equation, y = aebx, was fitted to the data of Figure 3-b. Where y is the complex viscosity of composites and x is filler volume fraction.
Filler a b R statistic
0.7 um Ba 1.22 6.81 0.983
0.5 um Silica 1.33 8.18 0.997
0.04 um Silica 8.38 10.39 0.992
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