Experimental and numerical study of optimum thickness of porous silica transition layer in aeronautic laminated glass

Accepted Manuscript Experimental and numerical study of optimum thickness of porous silica transition layer in aeronautic laminated glass

Zhijun Feng, Xufeng Wang, Juntong Huang, Xibao Li, Jinshan Lu PII: DOI: Reference:

S0264-1275(17)30196-X doi: 10.1016/j.matdes.2017.02.060 JMADE 2800

To appear in:

Materials & Design

Received date: Revised date: Accepted date:

8 December 2016 18 February 2017 18 February 2017

Please cite this article as: Zhijun Feng, Xufeng Wang, Juntong Huang, Xibao Li, Jinshan Lu , Experimental and numerical study of optimum thickness of porous silica transition layer in aeronautic laminated glass. The address for the corresponding author was captured as affiliation for all authors. Please check if appropriate. Jmade(2017), doi: 10.1016/ j.matdes.2017.02.060

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ACCEPTED MANUSCRIPT Experimental and numerical study of optimum thickness of porous silica transition layer in aeronautic laminated glass Zhijun Feng*, Xufeng Wang, Juntong Huang, Xibao Li, Jinshan Lu School of Material Science and Engineering, Nanchang Hangkong University,

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Nanchang, 330063, China *[email protected]

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Abstract: The application of a porous silica (PS) transition layer in an

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inorganic-organic aeronautic laminated glass can effectively solve the material failure

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caused by the performance difference of the inorganic-organic materials. The effect of porous silica transition layer thickness on the mechanical and optical properties of

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laminated glass was investigated. The microstructure of the porous silica transition layer was analyzed by scanning electron microscopy. The film thickness was verified using a

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step profiler. The failure strength of laminated glass with the porous silica transition layer was tested by a universal testing machine. Finite element modeling of laminated

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glass with the porous silica transition layer was performed by ANSYS software. Tensile stress between the porous silica and the polyurethane was simulated for different porous

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silica film thicknesses. Experimental and theoretical results indicated that with the increasing of the thickness of the transition film, the failure stress of the laminated glass increased. Improvements in the mechanical properties of the laminated glass are saturation at a PS thickness of approximately 3.8 μm. Keywords: Aeronautic laminated glass; Porous silica transition layer; Mechanical properties; Simulation 1. Introduction 1

ACCEPTED MANUSCRIPT Laminated glass has established its use as a structural material in airplanes windshield [1]. At present, due to the weight, the aeronautic laminated glass is mainly light organic laminated glass formed by two (or more) polymeric glass bonded by one (or more) thin polymeric interlayer(s), with a process at high temperature and pressure. However, in

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order to adapt to the marine climate environment (e.g., strong ultraviolet, high salt and high humidity), an inorganic-organic aeronautic windshield came into being [2].

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Inorganic glass (IG) as an outer layer can effectively resist ultraviolet and salt erosion

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[3]. Organic glass, usually polymethyl methacrylate (PMMA), as the inner layer can

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greatly reduce the weight of laminated glass. As the interlayer, polyurethane (PU) provides excellent properties such as the transparent property and good tear strength

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between the transparent materials such as IG and PMMA [4-9]. This failure mode has largely prevented the use of inorganic-organic laminated glass

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[10]. Peeling failure of the interface is one of the most common reasons why laminated glass is damaged without the influence of external factors [11]. The researchers found

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that peeling failure of laminated glass mainly occurs in the interface between the glass and the interlayer [12,13].

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A number of relevant studies on the structural performance of laminated glass, including static and dynamic loading, have been experimentally performed [14-16]. Biolzi et al. [17] tests by static and dynamic loading on laminated glass and assess their post-failure behavior. Andreozzi et al. [18] characterizes by dynamic torsion experiment the thermo-viscoelastic properties of polymeric interlayers for laminated glass. Numerical methods have been being intensively used to simulate the responses of laminated glass [19-25]. A finite element model with solid element could give the best 2

ACCEPTED MANUSCRIPT predictions of laminated glass responses. Larcher et al. [26] simulated laminated glass with an elastoplastic material model using dynamic testing data and elastic material model for glass. The mechanical properties of porous silica (PS) are intermediate between those of

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inorganic glass and organic polyurethane. When a transition layer of PS is inserted between the inorganic glass and organic polyurethane, it may help prevent interfacial

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failure [27]. As shown in the schematic of laminated glass featuring a silica transition

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layer with porous surface is in Fig. 1.

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The thickness of interlayer is one of the important factors affecting the mechanical properties of laminated glass [28-31]. At low porous silica transition layer thicknesses,

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the buffering effect of porous silica layer is not obvious. Conversely, if the layer thickness is too great, this may convert the three interdependent interfaces among IG, PS

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and PU into two new independent interfaces at IG/PS and PU/PS causing the interfacial cushioning effect to disappear. It is therefore important to identify a suitable thickness

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for the porous silica film layer.

In this paper, polymethyl hydrosiloxane (PMHS) and tetraethylorthosilica (TEOS)

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were used to prepare PS transition films with different thickness on inorganic glass [32-34]. Inorganic glass samples with PS transition films, polyurethane and PMMA were thermoformed to laminated glass. The effect of the PS film thickness on the mechanical behavior of the laminated glass was then investigated experimentally and by simulation. 2. Experiment and characterization 3

ACCEPTED MANUSCRIPT Commercial IG, PU and PMMA were obtained from Sinopharm Chemical Reagent Co., Ltd., Shanghai, China. The tensile strength of IG, PU and PMMA are 114.9 MPa, 48.2MPa and 110.5MPa at 20 ℃, respectively. The shear strength of PU is 16.7MPa. PS gel was prepared with a PMHS (MW≈1900, Aladdin):TEOS (99.99%, Aladdin) mass

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ratio of 1:2. A gel portion of 30, 60, 90 or 120 ml was deposited onto clean silicate glass (20 mm × 20 mm × 5 mm) by spin-coating at 2000 rpm. These films were then moved

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to a vacuum oven and dried for 8 h at 120 °C. The morphology of the PS transition

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films was observed by a JSM-5610LV scanning electron microscope (SEM, JEOL Ltd.,

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Japan). Film thickness was measured using a DEKTAK-150 step profiler (Veeco Instruments Inc., United States). The film thicknesses of samples A, B, C and D based

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on five measurement points were shown in Table 1, for the films cast with 30, 60, 90 and 120 ml of gel, respectively. Three layers of inorganic glass with a transition film,

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PU (15 mm × 20 mm × 3 mm) and PMMA (15 mm × 20 mm × 5 mm) were laminated by electric heating tablet machine. The bonding strength of the interface between the

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inorganic glass and PU was measured [3] by a WDW-50D universal test machine (Jinan Shijin Instrument Co., Ltd., China) on 3-ply unidirectional specimens, at a span to depth

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ratio of 5 according to GB/T 1450.1-2005. The forces applied to the laminated glass are shown in Fig. 2. The transparency were measured with a WGW photoelectric haze meter (Tianjin Optical Instrument Co., Ltd., China). The finite element modeling of laminated glass with different PS thicknesses performed by ANSYS software and is shown in Fig. 3. The sizes of the silica glass, PS film, PU and PMMA used in the finite element modeling were the same as those used to obtain the presented experimental data, which are shown in Table 2. Several different 4

ACCEPTED MANUSCRIPT film thicknesses were modeled: 0.0 μm, 1.0 μm, 2.0 μm, 3.0 μm, 3.2 μm, 3.4 μm, 3.6 μm, 3.8 μm, 4.0 μm, 5.0 μm and 6.0 μm. The pore diameter in the model was 0.75 μm from experimental data. Silica glass, PS, PU, and PMMA were simplified as elastic materials. Literature values of the mechanical properties (elastic modulus E, Poisson's

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ratio υ) of Silica glass, PS, PU, and PMMA in the model are shown in Table 3 [13,27]. Element type was SOLID 187.

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Boundary conditions and constraints are consistent with the schematic in Fig. 2. The

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displacement boundary condition and the force on the surfaces in the models are shown

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in Fig. 4. Force was applied to the IG and PS transition film at a rate of 1 N/s. Analysis type was transient analysis. When the modeled strain of any node in the laminated glass

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exceeded 0.035 from experimental data (See Fig. 6), the simulation is terminated.

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3. Results and discussion

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Fig. 5 displays an SEM image of the surface topography of a 3.58 μm thick PS transition layer. The surface of the transition film exhibited many open pores. The open

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pores were round, with diameters ranging from 0.5 μm to 1.5 μm, while most of the

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diameters were approximately 0.75 μm. A number of small pores were also distributed in the transition film, with a diameter of about 0.2 μm. The largest surface pores were likely formed by the aggregation of small pores in the silica gel, rose to the surface of the film and then ruptured during exposure to vacuum and high temperature. The surface morphologies of the PS films with different thicknesses were all similar to those shown in Fig. 5. Fig. 6 indicates stress-strain curves of laminated glass with PS transition layers of 5

ACCEPTED MANUSCRIPT different thicknesses under dynamic loading conditions. It is clear that the shear failure stress with a transition layer was larger than that without a transition layer. The shear failure stress was increased with the increasing of transition film thickness from 46.39 MPa without a transition film to 369.69 MPa when a 3.58 μm thick transition film was

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used, to a maximum value of 375.45 MPa when the transition film thickness was 4.27 μm. There were two reasons for the observed stress-strain behavior. During hot pressing,

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PU was pressed into the openings on the PS transition film surface. The interfacial

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structure therefore changed from an approximately two-dimensional smooth interface

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between IG and PU to a three-dimensional curved interface between PS and PU. As force was applied to the interface, the openings on the PS surface could cause a pinning

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effect, thus blocking shear stress. The mechanical properties of the transition film between IG and PU could also act as a buffer layer, causing less force to be transmitted

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to the PS/PU interface with increasing PS film thickness. This force buffering resulted in more shear stress being required to cause failure in an organic-inorganic composite

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laminated glass when using a PS transition film. Additionally, when the PS layer becomes excessively thick, the three-layer interface of IG, PS and PU were best

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described as a single interface rather than two independent interfaces at IG/PS and PS/PU. The interfacial bond strength between the IG and PS films is relatively small in the two independent interfaces. The interfacial failure in the samples with 3.58 μm and 4.27 μm thick PS films could thus occur at the IG/PS interface. Also from Fig.6, strains were not more than 0.035 as the sample shear was to failure. Fig. 7 shows an SEM cross-sectional images of the inorganic glass after the laminated glass composite with the transition layer was destroyed in the stress-strain experiments 6

ACCEPTED MANUSCRIPT discussed above. Seen from Fig. 7 (a), interfacial failure occurred in two main locations in the laminate glass with a PS film of 1.53 μm thickness. One point of failure was at the PS/PU interface where PU in the surface pores had been broken. Another point of failure was at the IG/PS interface where the PS film had been torn, as shown in the

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lower-right corner of Fig. 7 (a). This failure may be caused by too thin thickness of PS film with 1.53 μm, reducing the buffering effect of the transition film. Seen from Fig. 7

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(b), the interfacial failure occurred mainly at the PS/PU interface in laminate glass with

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a 2.64 μm thick PS film. However, the interfacial failure, in laminate glass with a 4.27

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μm thick PS film occurred at the IG/PS interface, where the entire PS film was peeled off (Fig. 7 (c)). Fig. 7 was thus consistent with our interpretation of the stress-strain data

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in Fig. 6.

Fig.8 shows the transmittance of laminated glass with the different thickness of

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transition film. As can be seen from Fig.8, the transmittance of laminated glass decreased rapidly with the increasing of film thickness. There were two reasons for this:

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on the one hand, with the increasing of the thickness, the absorption of the transition film increased; on the other hand, the small bubbles in the transition film would increase

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the scattering of light.

Fig. 9 is the experimental and simulated shear failure stress with different PS film thicknesses. It is apparent that with an increasing transition film thickness, the experimental and simulated failure stress rapidly increased and then plateaued at a constant value. This behavior can be explained using a similar analysis that was used to describe Figs. 6 and 7. Simulated failure stress was much larger than experimental failure stress. Because a perfect interface

was assumed in the model , i.e. no spatial 7

ACCEPTED MANUSCRIPT gaps among the PS, PU and IG. However, there is actually a slight gap between the three layers even after curing under vacuum. The data in Fig. 8 indicated that the mechanical properties of the glass were not improved when the PS transition layer thickness was increased beyond 3.8 μm. Increasing the PS layer beyond 3.8 μm would also further

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reduce the glass’s optical transmittance. A PS layer of approximately 3.8 μm therefore optimized the glass composite’s optical and mechanical properties by maximizing

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interfacial shear resistance while minimizing the thickness of the light-absorbing PS

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transition layer.

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Fig. 10 displays the simulated maximum interfacial stress of the IG/PS interface and the PS/PU interface at failure for laminated glass with different PS transition layer

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thicknesses. When the PS film thickness was 1 μm, the maximum stresses at the IG/PS

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interface and the PS/PU interfaces were both maximized as a function of PS film

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thickness and were close to their respective interface failure stress values. Failure occurred simultaneously at the IG/PS interface and the PS/PU interface. With the

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increasing of PS film thickness, the maximum stress at the IG/PS interface gradually decreased because of the buffering effect of the PS transition film. At this stage, failure

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occurred at the PS/PU interface. When the PS film thickness exceeded 3.2 μm, the maximum stresses at the IG/PS interface gradually increased and the maximum stress at the PS/PU interface gradually decreased. This behavior could be explained as the result of the three-component IG, PS and PU interface gradually separating into two independent interfaces, an IG/PS interface and a PS/PU interface, as the PS transition layer became thicker. At this stage, failure also occurred at the PS/PU interface. When 8

ACCEPTED MANUSCRIPT the PS film thickness exceeded 3.8 μm the maximum stress at the IG/PS interface gradually tended to the interface failure stress and the maximum stress at the PS/PU interface continually decreased. At this stage, failure occurred at the IG/PS interface. 4. Conclusion

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A PS film inserted between the IG and PU layer improved the shear resistance of

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laminated glass composites. Interfacial shear failure stress increased with the increasing of PS transition layer thickness before reaching a maximum value at a PS layer

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thickness of approximately 3.8 μm. When the PS transition film was too thin, failure

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simultaneously occurred at the IG/PS interface and the PS/PU interface, while the film

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was too thick, failure only occurred at the IG/PS interface. We have thus demonstrated the usefulness of incorporating a PS transition layer into laminated glass composites and

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used experimental and simulated data to explain the details of how the thickness of this

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layer affected the mechanical properties and failure behavior of the glass composites. The improved mechanical properties of the glass may make it a viable candidate for

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demanding applications such as aeronautical glass.

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Acknowledgments

The authors wish to acknowledge the National Natural Science Foundation of China (Grant No. 51302131) for the financial support.

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ACCEPTED MANUSCRIPT Figure Captions list Fig. 1 Schematic of laminated glass featuring a silica transition layer with porous surface. Fig. 2 Shear testing experimental setup on universal test machine. (a) shear testing

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specimen and device and (b) shear testing principles. Fig. 3 Finite element model diagram of laminated glass with the PS transition layer

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Fig. 4 Displacement and force boundary condition diagram on the model surfaces

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Fig. 5 SEM of the 3.58 μm thick PS film.

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Fig. 6 Stress-strain behavior under dynamic loading for laminated glasses with different film thicknesses.

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Fig. 7 SEM of the section on the inorganic glass with different film thickness: (a)1.53 μm, (b) 2.64 μm, (c) 4.27 μm

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Fig. 8 Transmittance of laminated glass with the different thickness of transition film Fig.9 Comparison of the experimental and simulated shear failure stress with different

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PS film thicknesses.

Fig.10 Maximum stress in IG/PS interface and PS/PU interface with different PS film

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thicknesses.

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ACCEPTED MANUSCRIPT Tables Table 1 The average film thicknesses of samples A, B, C and D /μm A

B

C

D

1

1.56

2.61

3.61

4.26

2

1.53

2.55

3.61

4.28

3

1.55

2.67

4

1.52

2.67

5

1.49

2.70

Average

1.53

2.64

0.027

0.060

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deviation

D

4.33

3.59

4.24

3.58

4.27

0.033

0.037

mm

PS

PU

PMMA

20

20

15

15

20

20

20

20

5

Variable

3

5

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Silica glass

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Thickness

3.55

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Table 2 Sizes of models

Width

4.24

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Standard

Length

3.54

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Simple

Table 3

E and n of the models

Silica glass

PS

PU

PMMA

E (GPa)

74.5

51.2

3.09

3.85

υ

0.25

0.26

0.47

0.32

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Graphical abstract

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ACCEPTED MANUSCRIPT Highlights 

Optimization mechanical and optical properties of laminated glass by adjusting PS layer thickness. Porous silica transition layer can improves shear resistance of laminated glass.

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Shear failure occurs at different interfaces when the film thickness is different.

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