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WITHDRAWN:Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites
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Data Article
Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites Xinhao Feng a,b, Zhaozhe Yang a, Qingwen Wang a,c, Siqun Wang b,n, Yanjun Xie a,n a Key Laboratory of Bio-Based Material Science and Technology (Ministry of Education), College of Material Science and Engineering, Northeast Forestry University, Harbin, Heilongjiang 150040, People’s Republic of China b Center for Renewable Carbon, University of Tennessee, Knoxville, TN 37996, United States c College of Materials and Energy, South China Agricultural University, Guangzhou, Guangdong 510640, People’s Republic of China
a r t i c l e i n f o
abstract
Article history: Received 12 April 2017 Received in revised form 30 December 2017 Accepted 4 January 2018
Various contents of lignin-coated cellulose nanocrystals (L-CNC) were incorporated into methacrylate (MA) resin and their mixture was used to prepare nanocomposites via 3D stereolithography (3D-SL) printing. A postcure was applied to further increase the properties of printed nanocomposites. In the data, the analyzed results on the mechanical and thermal properties of printed nanocomposites are presented. & 2018 Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Specifications Table Subject area More specific subject area Type of data
n
Material, Engineering, Additive manufacturing Material engineering, 3D printing Table, figure
DOI of original article: https://doi.org/10.1016/j.carbpol.2017.04.001 Corresponding authors. E-mail addresses: [email protected] (S. Wang), [email protected] (Y. Xie).
https://doi.org/10.1016/j.dib.2018.01.006 2352-3409/& 2018 Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
X. Feng et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
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55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108
How data was acquired Data format Experimental factors Experimental features Data source location Data accessibility
Tensile tests, SEM, NMR, FTIR, TGA, DSC and DMA were performed at University of Tennessee. Analyzed The mixture of L-CNC and MA was ultrasonicated, and the printed sample was postcured. 3 Replicates were used in TGA, DSC and DMA. The test sample was randomly cut from the printed sample. Knoxville, United States Data is with this article.
Value of the data
The method for fabrication the printed nanocomposites in this file is innovative and can be valuable to the industrial applications.
The printed material after postcure in this file with increased mechanical and thermal properties
could be potentially applied into package and tissue engineering where the high mechanical properties and thermal stability are needed. The data in this file plays a significant role for the researcher in further studies to describe the relationship between the properties of 3D-SL printed nanocomposites and postcure conditions, and to study the effect of lignin on the properties of 3D-SL printed nanocomposites.
1. Data The 3D-ST printing scheme and printing orientation are shown in Fig. 1. Rough and floppy-like surfaces and blunt layer edges were observed in the 3D-SL printed pure MA before postcure (Fig. 2a), and the smooth surface and pointy layer edges were observed in the postcured 3D-SL printed MA (Fig. 2b). Moreover, the gaps between MA matrix and L-CNC were gradually widened from 0.1% to 1% L-CNC content, and the holes generated by L-CNC pulling out from matrix were observed at high L-CNC contents (Figs. 2e and g). In Fig. 3, 1H NMR (a) and FTIR (b, c) spectra of 3D-ST printed L-CNC/MA nanocomposites before (b) and after (c) postcure were showed. Before postcure, both the tensile strength and tensile modulus increased slightly by the addition of
Fig. 1. 3D-ST printed L-CNC/MA nanocomposites, (a) schematic diagram of 3D-ST printing, (b) 3D-ST printing orientation of tensile specimen, and (c) tensile specimen of 3D-ST printed nanocomposites at different L-CNC content.
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 2. The fractural morphologies of 3D-ST printed L-CNC/MA nanocomposites at 0 wt% (a, b), 0.1 wt% (c, d), 0.5 wt% (e, f), and 1 wt% (g, h) L-CNC content before (a, c, e, and g) and after (b, d, f, and h) postcure.
0.1% L-CNC (Figs. 4a and b). Different from tensile strength and tensile modulus, the elongation decreased almost linearly with increasing of L-CNC content (Fig. 4e). The second maximum rate of weight loss temperature was not influenced by L-CNC (Tmax2 in Table 1, Fig. 5). L-CNC showed
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 3. 1H NMR (a) and FTIR (b, c) spectra of 3D-ST printed L-CNC/MA nanocomposites before (b) and after (c) postcure. (Raw MA: MA before printing; MA: printed neat MA before postcure; MA-C: printed neat MA after postcure; 0.5% L-CNC: printed MA with 0.5% L-CNC before postcure; 0.5% L-CNC-C: printed MA with 0.5% L-CNC after postcure).
one-step degradation, which started at 303.9 °C (5% weight loss) and obtained maximum rate of weight loss at 352.3 °C (Table 1). The DSC curves of the 3D-SL printed nanocomposites only showed a glass transition temperature (Tg) without a melting temperature (Fig. 6). At low temperature, the Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 4. Mechanical properties (a, b) tensile strength, (c, d) tensile modulus, and (e, f) elongation of non-postcured (a, c, and e) and postcured (b, d, and f) 3D-ST printed L-CNC/MA nanocomposites.
storage modulus of L-CNC/MA nanocomposites decreased compared to MA control (Fig. 7). The loss factors before and after postcure are shown in Fig. 8.
2. Experimental design, materials and methods 2.1. Materials L-CNC, purchased from American Process Inc. (USA), contains 3–6 wt% lignin, 0.052 wt% sulfur (ICP), and 4.3 wt% moisture, respectively. L-CNC was dried at 120 °C for 2 h before using. Photoreactive methacrylate (MA) resin (Clear Photopolymer Resin, model FLGPCL02), composed of monomer, oligomer, and photoinitiator, was supplied by Formlabs Inc. (USA). 2.2. L-CNC and MA resin compound processing The L-CNC at a content of 0, 0.1, 0.5, and 1 wt% was directly mixed with MA under stirring for 10 min, followed by an ultrasonication treatment at a power of 300 W for 6 min. The mixture was used as the raw material of 3D-SL printing. During printing, a laser beam, which was generated by the Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 5. TG (a, b) and DTG (c, d) of 3D-ST printed L-CNC/MA nanocomposites before (a, c) and after (b, d) postcure. Table 1 Temperature at 5% and 50% weight loss (T5% and T50%), maximum rate of weight loss temperature (Tmax1 and Tmax2) and glass transition temperature (Tg) of 3D-ST printed L-CNC/MA nanocomposites before and after postcure. L-CNC/ %
T5%/°C
Tmax1/°C
Before 0 0.1 0.5 1 100
288.9 291.4 292.8 288.2 303.9
7 7 7 7 7
After 0.2 0.4 0.3 0.5 0.2
296.9 303.9 301.8 296.6 –
7 7 7 7
0.3 0.2 0.6 0.3
Tmax2/°C
Before
After
359.6 7 0.5 364.8 7 0.2 365.7 7 0.7 361 7 0.3 352.3 7 0.6
359.5 367.3 367.5 367.2 –
Tg/°C
Before 7 7 7 7
0.6 0.2 0.4 0.3
454.9 453.9 454.1 452.7 –
7 7 7 7
After 0.3 0.4 0.6 0.5
451.3 7 456.5 7 458.9 7 455.7 7 –
Before 0.6 0.3 0.5 0.4
95.8 83.1 86.1 84.7 –
7 7 7 7
After 0.5 0.2 0.7 0.8
103.6 7 0.5 99.0 7 0.6 100.2 7 0.7 98.5 7 0.4 –
3D-ST printer (Form 1 þ, Formlab Inc., Cambridge, MA, USA), caused the chains of molecules linking together and solidified the liquid resin layer by layer until the final object was formed. The 3D-ST printing scheme and printing orientation are shown in Fig. 1. After printing, half of the 3D-ST printed samples were placed in the preheated oven (at 120 °C) and postcured for 40 min. 2.3. Scanning electron microscopy (SEM) The morphology of the fractured sample was studied by a scanning electron microscope (Zeiss Auriga SEM/FIB crossbeam workstation, Germany). Before observation, samples were dried and sputter-coated with gold. The accelerating voltage was 5 kV. 2.4. Nuclear magnetic resonance (NMR) characterization 1 H, gradient heteronuclear single quantum coherence (gHSQC) NMR measurement was carried out on a Varian 400-MR spectrometer equipped with a broadband probe operating at 399.78 MHz for
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 6. DSC diagrams of 3D-ST printed L-CNC/MA nanocomposites before (a) and after (b) postcure.
Fig. 7. Storage modulus of 3D-ST printed L-CNC/MA nanocomposites before (a) and after (b) postcure.
proton. 50 mg of sample was dissolved in 0.6 mL of acetone-d6. NMR spectra were recorded at 25 °C using the (HC)bsgHSQCAD pulse program. Acetone was used as an internal reference. 1H spectra were acquired with a 25 s relaxation delay, 2 scans, and an acquisition time of 2.556 s. The free induction decay (FIDs) were transformed using Mnova (Mestrelab Research SL., Santiago de Compostela, Spain). HSQC crosssignals were assigned by correlation with literature databases [1–5].
2.5. Fourier transform infrared spectroscopy (FTIR) analysis The FTIR analysis of 3D-ST printed L-CNC/MA nanocomposites was performed using a Perkin Elmer FTIR-ATR spectrometer (Spectrum One, Perkin Elmer, USA) at room temperature. Samples were placed on the diamond crystal of an attenuated total reflectance (ATR) accessory. Data were collected from 400 cm−1 to 4000 cm−1 with 20 scans for each sample. The resolution was 4 cm−1.
2.6. Tensile tests The tensile strength, modulus and elongation of 3D-ST printed L-CNC/MA nanocomposites were measured using a universal testing machine (Model 5567, Instron, Inc., Canton, MA) according to ASTM D638 [6]. The specimen is in a dogbone shape with dimension of 63.5 × 9.53 × 3.2 mm (L × W × T; the width of narrow section is 3.18 mm). Before testing, all samples were conditioned at 23 7 2 °C and 50 7 5% relative humidity for 24 h. Each type of formula was replicated 6 times at a crosshead speed of 1 mm/min. Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 8. The loss factor Tan δ of 3D-ST printed L-CNC/MA nanocomposites (dark line) with the Lorentz deconvolutions (colorfilled area) before postcure at 0 wt% (a, R ¼ 0.9909), 0.1 wt% (b, R ¼ 0.9886), 0.5 wt% (c, R ¼ 0.9900), and 1 wt% (d, R ¼ 0.9870) L-CNC content, and after postcure at 0 wt% (e, R ¼ 0.9807), 0.1 wt% (f, R ¼ 0.9844), 0.5 wt% (g, R ¼ 0.9875), and 1 wt% (h, R ¼ 0.9869) L-CNC content.
2.7. Thermo-gravimetric analysis (TGA) The thermal stability was determined using a thermal gravimetric analyzer (TGA, Perkin-Elmer 7 series, Perkin-Elmer Cetus Instruments, Norwalk, CT). The temperature range was from 25 °C to Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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433 600 °C using a heating rate of 10 °C/min in a dry atmosphere. Three tests were performed for each 434 sample. 435 436 2.8. Differential scanning calorimetry (DSC) 437 438 The thermal performance of the products was measured using a TA Q2000 (USA) differential scanning 439 calorimeter. The DSC specimens (approximately 2.5 mg) were sliced from the 3D-SL printed nano440 composites. Two temperature cyclic scans were taken under a 50 ml/min flow of nitrogen to prevent 441 oxidation. The first scan was to remove all residual moisture and erase any thermal history from 25 to 442 210 °C at a heating rate of 10 °C/min, and the specimen was held at 210 °C for 5 min. The samples were 443 then cooled to 25 °C at a rate of 10 °C/min and reheated to 210 °C at a heating rate of 10 °C/min. The 444 exothermic transition obtained from the second scan was termed the glass transition temperature (Tg). 445 446 2.9. Dynamic mechanical analysis (DMA) 447 448 Dynamic mechanical tests were performed with a dynamic mechanical analyzer (DMA Q800, TA 449 Instruments, New Castle, DE). Rectangular samples with dimensions of 55 mm × 13 mm × 2 mm were 450 3D-ST printed by the same compounds as the tensile test samples. Measurements were carried out in 451 the three-point bending mode by applying a constant 1 Hz frequency from −60 °C to 150 °C at a 452 heating rate of 3 °C/min from which the storage modulus (E’) and loss modulus (E’’) were obtained. 453 Three replicates were taken for each formula. 454 455 456 Acknowledgements 457 458 Financial supports from the Fundamental Research Funds for the Central Universities (Grant no. 459 2572015AB03 and no. 2572015AB23) and SMART (Soft Materials Research in Tennessee), Tennessee 460 Experimental Station Project #TEN00510 are gratefully acknowledged. The authors thank Dr. Stephen 461 Chmely and Dr. Kalavathy Rajan at The University of Tennessee, Center for Renewable Carbon for their 462 assistance of NMR data collection and analysis. 463 464 465 Transparency document. Supporting information 466 467 Q2 Transparency data associated with this article can be found in the online version at http://dx.doi. 468 org/10.1016/j.dib.2018.01.006. 469 470 471 References 472 473 [1] E. Klesper, A. Johnsen, W. Gronski, NMR study of configurational sequences in polymethacrylic acid, J. Polym. Sci. Part B: Polym. Lett. 8 (1970) 369–375. 474 [2] F. Biryan, K. Demirelli, G. Torğ ut, G. Pıhtılı, Synthesis, thermal degradation and dielectric properties of poly [2-hydroxy, 475 3-(1-naphthyloxy) propyl methacrylate], Polym. Bull. 74 (2017) 583-–602. 476 [3] M. Kostrzewska, B. Ma, I. Javakhishvili, J.H. Hansen, S. Hvilsted, A.L. Skov, Controlled release in hard to access places by poly (methyl methacrylate) microcapsules triggered by gamma irradiation, Polym. Adv. Technol. 26 (2015) 1059–1064. 477 [4] B. Fortier-McGill, V. Toader, L. Reven, 1H solid state NMR study of poly (methacrylic acid) hydrogen-bonded complexes, 478 Macromolecules 45 (2012) 6015–6026. 479 [5] P. Sahariah, B. Árnadóttir, M. Másson, Synthetic strategy for selective N-modified and O-modified PEGylated chitosan derivatives, Eur. Polym. J. 81 (2016) 53–63. 480 [6] ASTM D638-14 Standard Test Method for Tensile Properties of Plastics ASTM International, West Conshohocken, PA, 2014, 481 〈www.astm.org〉.
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Contents lists available at ScienceDirect
Data in Brief journal homepage: www.elsevier.com/locate/dib
Data Article
Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites Xinhao Feng a,b, Zhaozhe Yang a, Qingwen Wang a,c, Siqun Wang b,n, Yanjun Xie a,n a Key Laboratory of Bio-Based Material Science and Technology (Ministry of Education), College of Material Science and Engineering, Northeast Forestry University, Harbin, Heilongjiang 150040, People’s Republic of China b Center for Renewable Carbon, University of Tennessee, Knoxville, TN 37996, United States c College of Materials and Energy, South China Agricultural University, Guangzhou, Guangdong 510640, People’s Republic of China
a r t i c l e i n f o
abstract
Article history: Received 12 April 2017 Received in revised form 30 December 2017 Accepted 4 January 2018
Various contents of lignin-coated cellulose nanocrystals (L-CNC) were incorporated into methacrylate (MA) resin and their mixture was used to prepare nanocomposites via 3D stereolithography (3D-SL) printing. A postcure was applied to further increase the properties of printed nanocomposites. In the data, the analyzed results on the mechanical and thermal properties of printed nanocomposites are presented. & 2018 Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Specifications Table Subject area More specific subject area Type of data
n
Material, Engineering, Additive manufacturing Material engineering, 3D printing Table, figure
DOI of original article: https://doi.org/10.1016/j.carbpol.2017.04.001 Corresponding authors. E-mail addresses: [email protected] (S. Wang), [email protected] (Y. Xie).
https://doi.org/10.1016/j.dib.2018.01.006 2352-3409/& 2018 Published by Elsevier Inc. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
X. Feng et al. / Data in Brief ∎ (∎∎∎∎) ∎∎∎–∎∎∎
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55 56 57 58 59 60 61 62 63 64 65 66 67 68 69 70 71 72 73 74 75 76 77 78 79 80 81 82 83 84 85 86 87 88 89 90 91 92 93 94 95 96 97 98 99 100 101 102 103 104 105 106 107 108
How data was acquired Data format Experimental factors Experimental features Data source location Data accessibility
Tensile tests, SEM, NMR, FTIR, TGA, DSC and DMA were performed at University of Tennessee. Analyzed The mixture of L-CNC and MA was ultrasonicated, and the printed sample was postcured. 3 Replicates were used in TGA, DSC and DMA. The test sample was randomly cut from the printed sample. Knoxville, United States Data is with this article.
Value of the data
The method for fabrication the printed nanocomposites in this file is innovative and can be valuable to the industrial applications.
The printed material after postcure in this file with increased mechanical and thermal properties
could be potentially applied into package and tissue engineering where the high mechanical properties and thermal stability are needed. The data in this file plays a significant role for the researcher in further studies to describe the relationship between the properties of 3D-SL printed nanocomposites and postcure conditions, and to study the effect of lignin on the properties of 3D-SL printed nanocomposites.
1. Data The 3D-ST printing scheme and printing orientation are shown in Fig. 1. Rough and floppy-like surfaces and blunt layer edges were observed in the 3D-SL printed pure MA before postcure (Fig. 2a), and the smooth surface and pointy layer edges were observed in the postcured 3D-SL printed MA (Fig. 2b). Moreover, the gaps between MA matrix and L-CNC were gradually widened from 0.1% to 1% L-CNC content, and the holes generated by L-CNC pulling out from matrix were observed at high L-CNC contents (Figs. 2e and g). In Fig. 3, 1H NMR (a) and FTIR (b, c) spectra of 3D-ST printed L-CNC/MA nanocomposites before (b) and after (c) postcure were showed. Before postcure, both the tensile strength and tensile modulus increased slightly by the addition of
Fig. 1. 3D-ST printed L-CNC/MA nanocomposites, (a) schematic diagram of 3D-ST printing, (b) 3D-ST printing orientation of tensile specimen, and (c) tensile specimen of 3D-ST printed nanocomposites at different L-CNC content.
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 2. The fractural morphologies of 3D-ST printed L-CNC/MA nanocomposites at 0 wt% (a, b), 0.1 wt% (c, d), 0.5 wt% (e, f), and 1 wt% (g, h) L-CNC content before (a, c, e, and g) and after (b, d, f, and h) postcure.
0.1% L-CNC (Figs. 4a and b). Different from tensile strength and tensile modulus, the elongation decreased almost linearly with increasing of L-CNC content (Fig. 4e). The second maximum rate of weight loss temperature was not influenced by L-CNC (Tmax2 in Table 1, Fig. 5). L-CNC showed
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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163 164 165 166 167 168 169 170 171 172 173 174 175 176 177 178 179 180 181 182 183 184 185 186 187 188 189 190 191 192 193 194 195 196 197 198 199 200 201 202 203 204 205 206 207 208 209 210 211 212 213 214 215 216
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Fig. 3. 1H NMR (a) and FTIR (b, c) spectra of 3D-ST printed L-CNC/MA nanocomposites before (b) and after (c) postcure. (Raw MA: MA before printing; MA: printed neat MA before postcure; MA-C: printed neat MA after postcure; 0.5% L-CNC: printed MA with 0.5% L-CNC before postcure; 0.5% L-CNC-C: printed MA with 0.5% L-CNC after postcure).
one-step degradation, which started at 303.9 °C (5% weight loss) and obtained maximum rate of weight loss at 352.3 °C (Table 1). The DSC curves of the 3D-SL printed nanocomposites only showed a glass transition temperature (Tg) without a melting temperature (Fig. 6). At low temperature, the Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 4. Mechanical properties (a, b) tensile strength, (c, d) tensile modulus, and (e, f) elongation of non-postcured (a, c, and e) and postcured (b, d, and f) 3D-ST printed L-CNC/MA nanocomposites.
storage modulus of L-CNC/MA nanocomposites decreased compared to MA control (Fig. 7). The loss factors before and after postcure are shown in Fig. 8.
2. Experimental design, materials and methods 2.1. Materials L-CNC, purchased from American Process Inc. (USA), contains 3–6 wt% lignin, 0.052 wt% sulfur (ICP), and 4.3 wt% moisture, respectively. L-CNC was dried at 120 °C for 2 h before using. Photoreactive methacrylate (MA) resin (Clear Photopolymer Resin, model FLGPCL02), composed of monomer, oligomer, and photoinitiator, was supplied by Formlabs Inc. (USA). 2.2. L-CNC and MA resin compound processing The L-CNC at a content of 0, 0.1, 0.5, and 1 wt% was directly mixed with MA under stirring for 10 min, followed by an ultrasonication treatment at a power of 300 W for 6 min. The mixture was used as the raw material of 3D-SL printing. During printing, a laser beam, which was generated by the Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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271 272 273 274 275 276 277 278 279 280 281 282 283 284 285 286 287 288 289 290 291 292 293 294 295 296 297 298 299 300 301 302 303 304 305 306 307 308 309 310 311 312 313 314 315 316 317 318 319 320 321 322 323 324
Fig. 5. TG (a, b) and DTG (c, d) of 3D-ST printed L-CNC/MA nanocomposites before (a, c) and after (b, d) postcure. Table 1 Temperature at 5% and 50% weight loss (T5% and T50%), maximum rate of weight loss temperature (Tmax1 and Tmax2) and glass transition temperature (Tg) of 3D-ST printed L-CNC/MA nanocomposites before and after postcure. L-CNC/ %
T5%/°C
Tmax1/°C
Before 0 0.1 0.5 1 100
288.9 291.4 292.8 288.2 303.9
7 7 7 7 7
After 0.2 0.4 0.3 0.5 0.2
296.9 303.9 301.8 296.6 –
7 7 7 7
0.3 0.2 0.6 0.3
Tmax2/°C
Before
After
359.6 7 0.5 364.8 7 0.2 365.7 7 0.7 361 7 0.3 352.3 7 0.6
359.5 367.3 367.5 367.2 –
Tg/°C
Before 7 7 7 7
0.6 0.2 0.4 0.3
454.9 453.9 454.1 452.7 –
7 7 7 7
After 0.3 0.4 0.6 0.5
451.3 7 456.5 7 458.9 7 455.7 7 –
Before 0.6 0.3 0.5 0.4
95.8 83.1 86.1 84.7 –
7 7 7 7
After 0.5 0.2 0.7 0.8
103.6 7 0.5 99.0 7 0.6 100.2 7 0.7 98.5 7 0.4 –
3D-ST printer (Form 1 þ, Formlab Inc., Cambridge, MA, USA), caused the chains of molecules linking together and solidified the liquid resin layer by layer until the final object was formed. The 3D-ST printing scheme and printing orientation are shown in Fig. 1. After printing, half of the 3D-ST printed samples were placed in the preheated oven (at 120 °C) and postcured for 40 min. 2.3. Scanning electron microscopy (SEM) The morphology of the fractured sample was studied by a scanning electron microscope (Zeiss Auriga SEM/FIB crossbeam workstation, Germany). Before observation, samples were dried and sputter-coated with gold. The accelerating voltage was 5 kV. 2.4. Nuclear magnetic resonance (NMR) characterization 1 H, gradient heteronuclear single quantum coherence (gHSQC) NMR measurement was carried out on a Varian 400-MR spectrometer equipped with a broadband probe operating at 399.78 MHz for
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 6. DSC diagrams of 3D-ST printed L-CNC/MA nanocomposites before (a) and after (b) postcure.
Fig. 7. Storage modulus of 3D-ST printed L-CNC/MA nanocomposites before (a) and after (b) postcure.
proton. 50 mg of sample was dissolved in 0.6 mL of acetone-d6. NMR spectra were recorded at 25 °C using the (HC)bsgHSQCAD pulse program. Acetone was used as an internal reference. 1H spectra were acquired with a 25 s relaxation delay, 2 scans, and an acquisition time of 2.556 s. The free induction decay (FIDs) were transformed using Mnova (Mestrelab Research SL., Santiago de Compostela, Spain). HSQC crosssignals were assigned by correlation with literature databases [1–5].
2.5. Fourier transform infrared spectroscopy (FTIR) analysis The FTIR analysis of 3D-ST printed L-CNC/MA nanocomposites was performed using a Perkin Elmer FTIR-ATR spectrometer (Spectrum One, Perkin Elmer, USA) at room temperature. Samples were placed on the diamond crystal of an attenuated total reflectance (ATR) accessory. Data were collected from 400 cm−1 to 4000 cm−1 with 20 scans for each sample. The resolution was 4 cm−1.
2.6. Tensile tests The tensile strength, modulus and elongation of 3D-ST printed L-CNC/MA nanocomposites were measured using a universal testing machine (Model 5567, Instron, Inc., Canton, MA) according to ASTM D638 [6]. The specimen is in a dogbone shape with dimension of 63.5 × 9.53 × 3.2 mm (L × W × T; the width of narrow section is 3.18 mm). Before testing, all samples were conditioned at 23 7 2 °C and 50 7 5% relative humidity for 24 h. Each type of formula was replicated 6 times at a crosshead speed of 1 mm/min. Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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Fig. 8. The loss factor Tan δ of 3D-ST printed L-CNC/MA nanocomposites (dark line) with the Lorentz deconvolutions (colorfilled area) before postcure at 0 wt% (a, R ¼ 0.9909), 0.1 wt% (b, R ¼ 0.9886), 0.5 wt% (c, R ¼ 0.9900), and 1 wt% (d, R ¼ 0.9870) L-CNC content, and after postcure at 0 wt% (e, R ¼ 0.9807), 0.1 wt% (f, R ¼ 0.9844), 0.5 wt% (g, R ¼ 0.9875), and 1 wt% (h, R ¼ 0.9869) L-CNC content.
2.7. Thermo-gravimetric analysis (TGA) The thermal stability was determined using a thermal gravimetric analyzer (TGA, Perkin-Elmer 7 series, Perkin-Elmer Cetus Instruments, Norwalk, CT). The temperature range was from 25 °C to Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i
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433 600 °C using a heating rate of 10 °C/min in a dry atmosphere. Three tests were performed for each 434 sample. 435 436 2.8. Differential scanning calorimetry (DSC) 437 438 The thermal performance of the products was measured using a TA Q2000 (USA) differential scanning 439 calorimeter. The DSC specimens (approximately 2.5 mg) were sliced from the 3D-SL printed nano440 composites. Two temperature cyclic scans were taken under a 50 ml/min flow of nitrogen to prevent 441 oxidation. The first scan was to remove all residual moisture and erase any thermal history from 25 to 442 210 °C at a heating rate of 10 °C/min, and the specimen was held at 210 °C for 5 min. The samples were 443 then cooled to 25 °C at a rate of 10 °C/min and reheated to 210 °C at a heating rate of 10 °C/min. The 444 exothermic transition obtained from the second scan was termed the glass transition temperature (Tg). 445 446 2.9. Dynamic mechanical analysis (DMA) 447 448 Dynamic mechanical tests were performed with a dynamic mechanical analyzer (DMA Q800, TA 449 Instruments, New Castle, DE). Rectangular samples with dimensions of 55 mm × 13 mm × 2 mm were 450 3D-ST printed by the same compounds as the tensile test samples. Measurements were carried out in 451 the three-point bending mode by applying a constant 1 Hz frequency from −60 °C to 150 °C at a 452 heating rate of 3 °C/min from which the storage modulus (E’) and loss modulus (E’’) were obtained. 453 Three replicates were taken for each formula. 454 455 456 Acknowledgements 457 458 Financial supports from the Fundamental Research Funds for the Central Universities (Grant no. 459 2572015AB03 and no. 2572015AB23) and SMART (Soft Materials Research in Tennessee), Tennessee 460 Experimental Station Project #TEN00510 are gratefully acknowledged. The authors thank Dr. Stephen 461 Chmely and Dr. Kalavathy Rajan at The University of Tennessee, Center for Renewable Carbon for their 462 assistance of NMR data collection and analysis. 463 464 465 Transparency document. Supporting information 466 467 Q2 Transparency data associated with this article can be found in the online version at http://dx.doi. 468 org/10.1016/j.dib.2018.01.006. 469 470 471 References 472 473 [1] E. Klesper, A. Johnsen, W. Gronski, NMR study of configurational sequences in polymethacrylic acid, J. Polym. Sci. Part B: Polym. Lett. 8 (1970) 369–375. 474 [2] F. Biryan, K. Demirelli, G. Torğ ut, G. Pıhtılı, Synthesis, thermal degradation and dielectric properties of poly [2-hydroxy, 475 3-(1-naphthyloxy) propyl methacrylate], Polym. Bull. 74 (2017) 583-–602. 476 [3] M. Kostrzewska, B. Ma, I. Javakhishvili, J.H. Hansen, S. Hvilsted, A.L. Skov, Controlled release in hard to access places by poly (methyl methacrylate) microcapsules triggered by gamma irradiation, Polym. Adv. Technol. 26 (2015) 1059–1064. 477 [4] B. Fortier-McGill, V. Toader, L. Reven, 1H solid state NMR study of poly (methacrylic acid) hydrogen-bonded complexes, 478 Macromolecules 45 (2012) 6015–6026. 479 [5] P. Sahariah, B. Árnadóttir, M. Másson, Synthetic strategy for selective N-modified and O-modified PEGylated chitosan derivatives, Eur. Polym. J. 81 (2016) 53–63. 480 [6] ASTM D638-14 Standard Test Method for Tensile Properties of Plastics ASTM International, West Conshohocken, PA, 2014, 481 〈www.astm.org〉.
Please cite this article as: X. Feng, et al., Data on the mechanical and thermal properties of 3D printed nanocellulose reinforced methacrylate composites, Data in Brief (2018), https://doi.org/ 10.1016/j.dib.2018.01.006i