Core-shell encapsulation of PMHS@EPDM onto BF surface for strengthening and toughening of BF/HDPE composites

doi:10.21203/rs.3.rs-2019768/v1

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Core-shell encapsulation of PMHS@EPDM onto BF surface for strengthening and toughening of BF/HDPE composites

https://doi.org/10.21203/rs.3.rs-2019768/v1

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published 19 May, 2023

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Bamboo flour/high-density polyethylene (BF/HDPE) composite was strengthened and toughened simultaneously by the surface encapsulation of BF with poly(methylhydrogen)siloxane(PMHS) and Ethylene Propylene Diene Monomer (EPDM). An elastic PMHS@EPDM shell was fabricated on BF surface by successively spraying PMHS/hexane and EPDM/hexane solutions onto BF, based on the dehydrogenation and addition reaction of PMHS with BF and EPDM. It was found that surface encapsulation of wood at high PMHS content would simultaneously increase the strength and toughness of BF@PMHS/HDPE composite. The tensile strength and impact strength were increased by 54.2% and 9.9%, respectively as PMHS content was 3.3%. Furthermore, an encapsulation of BF@PMHS with EPDM further increased the strength and toughness by 5.1% and 14.7%. Compared with the pristine BF/plastic composites (BPC), the tensile, flexural and impact strength of modified BPC increased by 62.1%, 28.0% and 26.1%. The changes in the microstructure of the interface between BF and HDPE as a function of encapsulation of PMHS and EPDM and the relationship between chemical structure, microstructure and mechanical properties were discussed in detail. This work gave a novel MAH-free method for strengthening and toughening BF/HDPE or wood flour/high-density polyethylene (WF/HDPE) composites.

Poly(methylhydrogen)siloxane

Natural fiber composites

Mechanical properties

Surface treatments

Shell theory

Synergism

Chinese President Xi stated at the 75th Session of the United Nations General Assembly that China will strive to achieve carbon dioxide peak by 2030 and carbon neutrality by 2060. With the rapid development of the bamboo industry in China, a large number of bamboo flour (BF) are produced as residual yearly. Most of them are incinerated and landfilled as fuel or fertilizers, resulting in environmental damage and releasing a large amount of greenhouse gases. Obviously, this is not conducive to the response to carbon peaking and carbon neutrality policies. Consequently, these residuals of bamboo processing must be used in a green way. The application of BF in preparation of BF/plastic composites (BPC) opens up new field for reducing carbon emissions as an environmentally friendly material (Liu et al 2022; Liu et al 2016; Zhang et al 2018). BPC can replace wood and bamboo as decoration materials; therefore, BPC will reduce the disafforestation and incineration or landfill of BF. However, there is a critical problem for BPC, which is well-known as poor interface compatibility between BF and polymer matrix (Bai et al 2021; Dun et al 2021). This is because polymer is generally hydrophobic, while BF is very hydrophilic due to the amounts of hydroxyl groups on its surface (Aouat et al 2020). Therefore, it is highly desirable to increase the interfacial compatibility to improve the mechanical properties of BPC. Many methods, which could be summarized as physical modification (Alekseeva et al 2021; Faruk et al 2012; Jiajia et al 2019), chemical modification (Bland et al 2019; Chen et al 2018; Hung et al 2012; Lei et al 2017; Reddy et al 2013; Seo et al 2020; Wang et al 2010), and physical and chemical combined modification (Mei et al 2016; Ndazi et al 2007; Ning et al 2019; Yu et al 2019), have been reported. These methods generally focused on strengthening of BPC. In addition, there were also much research about the toughening BPC (Cai et al 2011; Qian et al 2018). However, strength and toughness of BPC are generally contradictory, and often the enhancement of one property is at the expense of the other (Ritchie 2011; Yang et al 2019).

Therefore, most research has been devoted to optimizing the strength-toughness balance. Fortunately, in this progress, an effective method has been gradually developed for simultaneous improvement of strength and toughness, which can be defined as the maleic anhydride (Reddy et al) grafted method. The MAH grafted method can be divided into three methods. The first one is the addition of MAH grafted polymer which is the same as the matrix, such as MAH-g-PE (MAPE), MAH-g-PP (MAPP) to the composites (Chow et al 2003; Garcia-Garcia et al 2016; Sombatsompop et al 2005; Stefani et al 2021). This method can generally improve the strength of composites with a slight improvement in toughness. To improve the toughness of composites, the second method replaced the matrix polymer with elastomers. Adding MAH grafted elastomers (such as MAH-g-EPR, MAH-g-EPDM, MAH-g-SEBS) into composites can greatly increase the toughness (And and Lindberg 1998; Guo et al 2007; Hsieh et al 2016; Jiang et al 2004). However, the strength of the composites was not satisfactory. Therefore, the third method tried to combine the first and second methods to simultaneously increase the strength and toughness to a great extent (Ao et al 2007; Liu et al 2008; Wu et al 2000). Until now, few MAH-free methods have been reported to improve strength and toughness simultaneously.

In our previous work, PMHS was used for surface hydrophobic modification of BF to improve the mechanical properties of BPC (Xiao et al 2021). The most interesting finding was that PMHS could play contrary roles in adjusting the mechanical properties, in which PMHS with backbone structure of -[Si(H)CH₃-O]_m- serve as a hard interface layer between BF and HDPE while that of -[Si(H)CH₃-O]_m-[Si(CH₃)₂-O]_n- played as a soft interface layer. The former increased the strength but decreased the toughness, while the latter increased the strength and toughness simultaneously. Although both the strength and toughness were not improved satisfactorily, it gave us an idea that the strength and toughness of BPC can probably improve simultaneously as a soft and hydrophobic layer with low crosslinking density was built onto the BF surface.

In this work, a two-step surface modification and MAH-free method were investigated for simultaneous enhancement of strength and toughness of BF/HDPE composites by fabricating crosslinked elastic PMHS@EPDM shell onto BF surface. In the first step, based on the dehydrogenation between -Si-H of PMHS and –OH of BF, PMHS chains were grafted onto BF surface to fabricate BF@PMHS, incorporating lots of reactive -Si-H groups onto BF for subsequent modification. In the second step, BF@PMHS@EPDM with a elastic PMHS@EPDM shell was fabricated based on the addition reaction between vinyl groups of EPDM and -Si-H groups of BF@PMHS. Compared with the pristine BPC, the tensile strength and impact strength of modified BPC were simultaneously increased by 62.1% and 26.1%. Finally, the mechanism for effect of the elastic PMHS@EPDM layer between BF and HDPE on the mechanical properties of BF/HDPE composites was discussed in detail. This work aims to give a novel route for strengthening and toughening BPC or WPC.

Materials

Bamboo flour (BF) with an average particle size of 220 µm was given by Jiangsu Straw processing Industry (Jiangsu, China). HDPE was provided by PetroChina Company Limited (1103-3B). PMHS with a reactive hydrogen content of 1.5% and Kastredt catalyst (platinum-1, 3-divinyl-1,1,3,3-tetramethyldisiloxane) with Pt content of 2000 ppm were obtained from Chenguang Research Institute of Chemical Industry (Chengdu, China). EPDM (Nordel 4725) was obtained from Dow Chemical company. EPDM (Nordel 4725, Dow Chemical) with the ethylene, propylene and ethylidene norbornene content of 70, 25 and 5 wt.%, respectively was used. N-hexane was purchased from Tianjin Zhiyuan Chemical Reagent Co., Ltd.

Preparation Of Bf@pmhs

50 g n-hexane, 0.1 g Kastredt catalyst and PMHS of different quality were mixed together and then sprayed onto 90 g pristine BF to prepare BF@PMHS. The content of PMHS varied from 0.0–3.3%.

Preparation Of Bf@pmhs@epdm

EPDM with different quality was dissolved in 50 g n-hexane, and then sprayed onto 80 g BF@PMHS. The resultant BF was named as BF@PMHS@EPDM, and the content of EPDM varied from 0.0–2.4%.

Preparation Of Bf/hdpe Composites

80 g BF (pristine or BF@PMHS, BF@PMHS@EPDM) and 320 g HDPE were mixed by an internal mixer (Bolon Precision Testing Machines Corporation, Guangdong, China) at 180℃ and 50 r/min screw speed for 15 min. The bulk BPC was crushed into small particles by PC-400A strong plastic crusher and then put into a 100 ℃ oven to dry for 3 hours. Finally, they were processed into standard samples for subsequent characterization and mechanical property testing with an injection molding machine (Haiying Plastics Machinery Co., LTD, Ningbo, China) .

Characterization

The chemical properties of pristine BF, BF@PMHS and BF@PMHS@EPDM were characterized by Fourier transform infrared spectroscopy (FTIR, Bruker Tensor 27) and EDS (Oxford X-Max N), respectively. The FTIR spectra were recorded by KBr pellet method, with a scan range of 4000 cm^− 1 to 400 cm^− 1 at a resolution of 4 cm^− 1 for 32 scans. The water contact angles (WCA) was tested with contact angle measuring instrument (HARKE-SPCA-1). Before the WCA test, the samples were pressed with a powder tablet machine at 30 MPa for 20 s into flakes, and then 5 µL of distilled water was dropped onto the surface of the above flakes, and the test was performed after standing for several seconds.

The tensile and flexural properties of the composites were tested with a universal testing machine (CMT6014) following GB/T1040-92 and GB/T9341-2000, respectively. Both tensile and flexural properties were tested at a rate of 10 mm/min, the gauge length for tensile properties was 50 mm, and the span for flexural testing was 60 mm.

The impact strength test was tested according to GB/T1043-93. The samples were injection molded into notched rectangular samples (80 × 10 × 4 × 1mm³, Notch depth: 1mm), carried out on an impact testing machine (ZBC7251-B). For the mechanical properties experiments of the composites, each sample was tested five times. Morphology of impact fractured surface was tested by scanning electron microscopy (SEM, ZEISS Z500). A thin layer of gold was sputtered onto the surface of the sample prior to testing to improve conductivity.

Chemical properties and morphology of BF

The encapsulation of PMHS and EPDM onto BF surface can be verified by FTIR and SEM-EDS analyses. Figure 1 shows the FTIR spectra of pristine BF, extracted BF@PMHS and BF@EPDM@PMHS. Compared with the pristine BF, BF@PMHS presented additional absorption peaks at 2968 cm^− 1, 2164 cm^− 1 1106 cm^− 1 and 767 cm^− 1, which are attributed to the -Si-CH₃, -Si-H and -Si-O-Si groups of PMHS, respectively (Lin et al 2020). In addition, BF was intentionally immersed into PMHS/hexane/catalyst solution, and many bubbles were observed, which is attributed to the ultra-high reactivity of -Si-H of PMHS with -OH groups on BF surface with Kastredt catalyst (Lin et al 2018). This phenomenon combined with results of FTIR characterization indicates that PMHS is successfully grafted on the surface of BF by the dehydrogenation between -Si-H of PMHS and -OH of BF. For BF@EPDM@PMHS, there was an additional absorption peak at 2850 cm^− 1, attributed to -CH₂- of EPDM (Ashok et al 2020). Furthermore, the intensity at 2165 cm^− 1 decreased, indicating that EPDM was encapsulated onto BF@PMHS surface by the addition reaction between -Si-H of BF@PMHS and vinyl groups of EPDM.

To demonstrate the encapsulation of PMHS and EPDM onto BF surface, the surface morphology and chemical properties of pristine BF, BF@PMHS and BF@PMHS@EPDM were characterized by SEM-EDS. The bamboo processing process produced lots of longitudinal cracks and corrugations at BF surface, which were observed clearly in Fig. 2 (a). After encapsulating PMHS and EPDM onto BF surface, as shown in Fig. 2 (b, c), these cracks were covered by PMHS or PMHS@EPDM shell. Results from EDS, (Fig. 2a1, b1, c1) were in good agreement with those of FTIR. There were only C and O elements for pristine BF with atom percent of 58.56% and 41.44%, respectively. After PMHS modification, the characteristic element (Si) of PMHS was recorded with an atom percent of 0.96%, indicating the incorporation of the PMHS shell onto BF surface. As shown in Fig. 2 (c), the atom percent of C increased slightly due to the encapsulation of EPDM onto BF surface, demonstrating that BF@PMHS was further covered by EPDM.

The change in chemical properties of BF after encapsulation of PMHS and EPDM was also recorded as shown in Fig. 2 (a2, b2, c2). Pristine BF, BF@PMHS and BF@PMHS@EPDM were put on the glass slide with double-side tape for water contact angle characterization. As shown in Fig. 2 (a2), the water droplet could be easily absorbed by pristine BF; therefore, the water contact angle is very low. In addition, after pouring pristine BF onto water, it sank into water because it was very hydrophilic. As shown in Fig. 2 (b2, c2), the water droplets were difficult to adhere onto BF@PMHS and BF@PMHS@EPDM, and the water contact angles were both higher than 150°, indicating a good encapsulation of PMHS and EPDM shell that is of low surface energy onto BF. In addition, BF encapsulated by PMHS and PMHS@EPDM was difficult to sink into the water.

Mechanical Properties Of Bf@pmhs/hdpe Composites

Tensile and flexural strength

Figure 3 shows the measured tensile strength, flexural strength and impact strength of BF/HDPE composites as a function of PMHS concentration. The tensile strength of pristine BF/HDPE composite is 21.3 MPa, which is lower than that of pure HDPE (26.7 MPa). The large difference in polarity between hydrophilic BF and hydrophobic HDPE leads to the poor interfacial adhesion. SEM characterization of the impact-fractured surface is an effective method for providing insight into information related to interfacial adhesion. Figure 4 (a, b) shows the morphology of impact-fractured surfaces of BF/HDPE. Very poor compatibility and interface bonding between HDPE and BF could be concluded because many caves and clear cracks between BF and HDPE were observed. Therefore, the energy and stress transfer of HDPE/BF composites was of little effectiveness.

For BF@PMHS/HDPE composites, as shown in Fig. 3, the tensile strength and flexural strength increased significantly with PMHS content. As PMHS content increased from 0.0–3.3%, composites' tensile strength and flexural strength increased gradually from 21.3 MPa to 32.8 MPa and from 30.1 MPa to 39.8 MPa, respectively, indicating that the interfacial adhesion between BF and HDPE is significantly improved. Figure 5 (b) showed the reaction mechanism between PMHS and BF and the strengthening mechanism of PMHS in BF@PMHS/HDPE composites. As shown in Fig. 5 (a), PMHS is consisted of –SiCH₃(H)-O- units with two end groups of -Si(CH₃)₃. PMHS is well-known for its ultra-high reactivity of –Si-H at room temperature with the aid of Kastredt catalyst and its very low surface energy (Zhang et al). As PMHS/hexane solution with Kastredt catalyst was sprayed onto BF surface at room temperature, -Si-H of PMHS reacted immediately with -OH groups on BF surface, and PMHS chains with low surface energy were covalently grafted onto BF surface by the dehydrogenation. The surface of BF transformed gradually from hydrophilic to very hydrophobic, and the difference in polarity between BF and HDPE was removed by PMHS modification of BF. Therefore, the interfacial adhesion between BF and HDPE and hence the tensile and flexural strength improved gradually with PMHS content. This is demonstrated vividly by the SEM images of impact-fractured surfaces of BF@PMHS/HDPE composite, as shown in Fig. 4(c, d, e, f). At low PMHS content of 0.2%, there were also clear cracks between BF and HDPE matrix. However, less BF was pulled out from the matrix, and smaller gaps between BF@PMHS and HDPE were found. Most importantly, many HDPE were observed directly to adhere to BF, indicating an improvement in compatibility and bonding between HDPE and BF.

As PMHS content is increased to 3.3%, there is no visible crack between BF and HDPE, indicating the excellent interfacial adhesion between BF and HDPE. Figure 4(e, f) also showed many BF with glossy surface, revealing that BF was broken during impact test rather than being pulled out from HDPE matrix. Furthermore, transition zones were found between BF and HDPE matrix, which was probably evidence of the interface’s struggling progress to the applied force. It was well-known that HDPE was packed by fold chains. Due to the excellent interfacial bonding between HDPE and BF@PMHS, the fold chains were straightened during the impact test, which was vividly observed in the transition zone.

Impact Strength

As shown in Fig. 3, PMHS played different roles in adjusting the toughness of BF/HDPE composite at low and high PMHS content. As PMHS content increased slightly from 0.0–0.2%, the impact strength decreased from 16.1 MPa to 13.4 MPa. This was in accordance with our published work and most other people’s research about strengthening BF/HDPE composites, in which the strengthening of composites is at the expense of toughness. In this work, we intentionally increased PMHS content to afford abundant –Si-H groups onto BF surface for further crosslinking with EPDM. As PMHS content increased gradually from 0.2–3.3%, the impact strength increased greatly from 13.4 MPa to 17.7 MPa.

To explain the role of PMHS in adjusting the toughness of BF/HDPE composites, two different encapsulation manners of BF with PMHS at low and high PMHS content were drawn and represented in Fig. 5. Considering the steric effect, Si-H groups at the end of PMHS chains possess much higher reactivity. Therefore, PMHS chains tended to be grafted onto BF surface by the dehydrogenation of the end –Si-H group of PMHS chains and -OH groups on BF surface.

At low PMHS content, a small quantity of PMHS chains is grafted onto BF surface. Due to the excellent flexibility of PMHS chains, the internal rotation of PMHS chains made most units of PMHS attach to BF surface, and the units with –Si-H groups would react with hydroxyl groups of BF. Therefore, there is only a very thin PMHS shell on BF. Although PMHS chains possessed excellent flexibility, the thin PMHS shell on BF surface would be very rigid. The rotation of PMHS chain segments was limited because they were covalently bonded onto BF. The thin and rigid PMHS shell gave BF@PMHS/HDPE composites improved strength but worse toughness.

At high PMHS content, large numbers of PMHS chains were grafted onto BF surface. As shown in Fig. 5, only the Si-H end groups of PMHS reacted with –OH groups of BF, and the rotation of PMHS segments was freer. Therefore, encapsulation of BF at high PMHS content gave a thick and soft PMHS layer on BF surface, affording BF@PMHS/HDPE composites improved toughness.

Mechanical Properties Of Bf@pmhs@epdm/hdpe Composites

Based on the above discussion, we summarized the methods and the key requirements for simultaneous improvement of strength and toughness. The methods could be divided into two categories: surface modification of BF and addition of toughening agent. Both required two key factors: one is that the modifiers or toughening agent should have low surface energy and good flexibility, and the other is that the surface modifier or toughening agent should be covalently grafted onto BF surface. According to the references, most reported methods just meet one requirement. For example, silane coupling agents with the chemical structure of R-Si(OR’)₃ were used for hydrophobic modification of BF or WF to strengthen BPC or WPC. However, because the hydrophobic groups of -R were generally short alkyl chains, which could not create a thick and soft layer on BF or WF surface, the toughness was almost decreased. The other typical example is the addition of EPDM to BPC or WPC for toughening them. EPDM was well-known for its excellent flexibility, and therefore it would greatly improve the toughness of BPC or WPC but obviously decrease the strength. Actually, EPDM is of low surface energy. Supposing that EPDM was covalently encapsulated onto BF or WF surface, the strength and toughness would increase simultaneously. However, EPDM is dispersed uniformly in the polymer matrix, which was of little help in improving the interfacial adhesion between filler and polymer matrix.

As previously discussed (as shown in Fig. 3), encapsulation of PMHS at high content improved strength and toughness simultaneously, in which the tensile strength was increased by 54.2%, while the impact strength was only increased by 9.9%. A second step encapsulation of BF@PMHS with EPDM was proposed based on the addition reaction between -Si-H groups of BF@PMHS and vinyl groups of EPDM. Our original idea for this work is to optimize the trade-off between strength and toughness of BPC by controlling the cross-linking degree of PMHS-EPDM shell on BF surface. We have conceived that the second step would increase the toughness greatly at the expense of a very modest decrease in strength. However, to our surprise, as shown in Fig. 6, the encapsulation of EPDM to PMHS@BF increases both the toughness and the strength. As shown in Fig. 6, as EPDM content increased from 0.0–2.4%, the tensile strength and impact strength increased from 32.8 MPa to 34.5 MPa and from 17.7 MPa to 20.3 MPa, respectively, which increased by 5.1% and 14.7% compared with BF@PMHS/HDPE composites. This is attributed to the interesting chemical structure of BF, PMHS and EPDM and the reaction between them. Generally speaking, the addition of EPDM to BF/HDPE composites decreased the strength due to the excellent flexibility of EPDM. However, in this work, in addition to working as toughening agent, EPDM also played the role of cross-linker with PMHS chains on BF@PMHS. The cross-linking between PMHS was helpful to the tensile strength, and therefore the strength increased slightly even though EPDM was added. At the same time, because the crosslinking density was probably low, the rotation of chain segments of PMHS and EPDM was only limited slightly. Hence, the impact strength increased by a further encapsulation of EPDM onto BF@PMHS. As shown in Fig. 4(g, h), there was a few cracks between HDPE and BF@PMHS@EPDM and BF was split rather than pulled out, revealing good compatibility. The morphology of the interface between BF and HDPE was different from that of HDPE/BF@PMHS. Many wires were extended from the interface, attributed to the elongation of EPDM chains. Finally, EPDM wires were extended from HDPE matrix because there were also some free EPDM chains in the matrix.

The simultaneous enhancement of strength and toughness of BF/HDPE composites was studied by fabricating elastic PMHS@EPDM shell onto BF surface in a two-step surface modification and MAH-free method. The modifications were based on the dehydrogenation between -Si-H of PMHS and -OH of BF, in the first step, and the addition reaction between vinyl groups of EPDM and -Si-H groups of BF@PMHS with an elastic PMHS@EPDM shell in the second step. FTIR and SEM-EDS characterization of pristine and modified BF demonstrated the encapsulation of BF with PMHS and EPDM. Encapsulation manner was controlled by simply adjusting PMHS content. PMHS encapsulation at high PMHS content simultaneously improved the tensile and impact strength of BF@PMHS/HDPE composites by 54.2% and 9.9%, respectively. The excellent interfacial bonding between BF@PMHS and HDPE was observed in SEM image, in which HDPE chains were straightened at the surface of BF to form a transition zone. Furthermore, an encapsulation of BF@PMHS with EPDM further increased the strength and toughness by 5.1% and 14.7%.

Acknowledgements

The authors gratefully acknowledge the support from the Leading Project of Fujian Province of China (2019H0008), and Innovation Fund project of Fujian Agriculture and Forestry University (KFA19113A).

Conflict of interests

The authors declare that there is no conflict of interest regarding the publication on this paper.

Author contributions

Tao Wen wrote the main manuscript text and prepared figures; Xinxiang Zhang revised the main manuscript text and gave experimental guidance; Kehinde Olonisakin revised the main manuscript text; Sainan Ou and Fuchuan Xiao did experiments. And all authors reviewed the manuscript.

Funding

The authors gratefully acknowledge the support from the Leading Project of Fujian Province of China (2019H0008), and Innovation Fund project of Fujian Agriculture and Forestry University (KFA19113A).

Ethics approval and consent to participate: Not applicable

Consent for publication

All the authors gave their consent and agreed that this article to be published in cellulose journal.

Availability of data and materials

The data for this research are available upon request from the authors

Author’s information: Not applicable

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No competing interests reported.

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Journal Publication

published 19 May, 2023

Read the published version in Cellulose →

Editorial decision: Major revision
23 Feb, 2023
Reviews received at journal
17 Dec, 2022
Reviewers agreed at journal
06 Dec, 2022
Reviewers invited by journal
30 Sep, 2022
Editor assigned by journal
20 Sep, 2022
Submission checks completed at journal
16 Sep, 2022
First submitted to journal
31 Aug, 2022

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Core-shell encapsulation of PMHS@EPDM onto BF surface for strengthening and toughening of BF/HDPE composites

Status:

Journal Publication

Version 1

Abstract

Figures

Introduction

Experimental

Materials

Preparation Of Bf@pmhs

Preparation Of Bf@pmhs@epdm

Preparation Of Bf/hdpe Composites

Characterization

Results And Discussion

Chemical properties and morphology of BF

Mechanical Properties Of Bf@pmhs/hdpe Composites

Tensile and flexural strength

Impact Strength

Mechanical Properties Of Bf@pmhs@epdm/hdpe Composites

Conclusions

Declarations

References

Additional Declarations

Status:

Journal Publication

Version 1