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Mechanical Property Regulation of Graphene Oxide Separation Membranes

Binbin Zhu , Xiaohui Zheng , Guang Yang , Xu Zeng , Wei Qiu , Bin Xu

Progress in Chemistry ›› 2021, Vol. 33 ›› Issue (4) : 670 -677.

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Progress in Chemistry ›› 2021, Vol. 33 ›› Issue (4) : 670-677 DOI: 10.7536/PC200459
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Mechanical Property Regulation of Graphene Oxide Separation Membranes
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Abstract

Due to the controllable nanoscale channels and unique separation performance, the separation films assembled from graphene oxide(GO) nanosheets are promising separation materials, but the unsatisfactory mechanical properties restrict their practical application. Introducing particles such as active molecules and cations between the GO nanosheets can improve the mechanical properties of the GO membranes due to the formation of the stable bonding. In this review, the recent progress on the methods for improving the mechanical properties of GO membranes is summarized. According to the bonding mode between GO and the introduced particles, these methods can be divided into two types, covalent bonding and non-covalent bonding. Furthermore, covalent bonding methods can be divided into macromolecular covalent bonding and small molecule covalent bonding, while noncovalent bonding methods include hydrogen bonding, π-π bonding and ionic bonding. Both covalent bonding and noncovalent bonding can significantly improve the mechanical properties of the GO films, while the covalent bonding methods are more effective. Among the covalent bonding methods, the macromolecule covalent bonding is superior to the small molecule covalent bonding. Finally, the major problems of the current methods for enhancing the mechanical property of GO are discussed, and the future prospects is proposed.

Content:

1 Introduction

2 Covalent bonding method

2.1 Small molecule covalent bonding method

2.2 Macromolecular covalent bonding method

3 Noncovalent bonding method

3.1 Ionic bonding method

3.2 Hydrogen bonding method

3.3 π-π bonding method

4 Conclusion and prospect

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Keywords

670/img_1.png509.95253.9graphene oxide membranes / mechanical properties / covalent bonding / noncovalent bonding

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Binbin Zhu, Xiaohui Zheng, Guang Yang, Xu Zeng, Wei Qiu, Bin Xu. Mechanical Property Regulation of Graphene Oxide Separation Membranes. Progress in Chemistry, 2021, 33(4): 670-677 DOI:10.7536/PC200459

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1 Introduction

Graphene oxide (GO) is a novel two-dimensional nanomaterial, which contains a large number of oxygen-containing functional groups such as hydroxyl and carboxyl groups on its surface. The GO sheet layer can be formed into a film by vacuum filtration, suspension coating, spray coating, layer-by-layer self-assembly, blending assembly and other methods, and the GO film formed by stacking the GO nano sheets layer by layer contains abundant nano channels[1⇓~3]. The process of molecular permeation through the GO membrane can be regarded as the flow of molecules along the smooth and low-friction two-dimensional capillary channels of graphene. According to the size sieving theory, when the radius of molecules or ions is larger than the size of the nano-channel of the separation membrane, they can not pass through the separation membrane to achieve selective rejection of the membrane[4,5]. Therefore, GO membrane can effectively intercept and separate the solute particles in the solution, so as to realize the separation of liquid and mass, and can be applied to the fields of sewage filtration, gas barrier and seawater desalination[6⇓~8].
Because of its unique nano-layered structure, abundant functional groups and good hydrophilicity, GO membrane is considered to be a promising separation membrane material and has become a hot research topic at home and abroad[9]. In 2012, Nair et al. Prepared a GO film with a thickness of micron by spin coating, which can effectively block gases (including helium, hydrogen, nitrogen, etc.) And organic solvent vapors, but water molecules can penetrate through without hindrance, indicating that GO film has potential selective separation[10,11]. In 2014, Nair et al. Further studied the mass transfer characteristics of GO membrane and found that the tightly stacked GO membrane can be regarded as a capillary network with two-dimensional nanochannels, and the capillary pressure inside the GO membrane makes water molecules and ions in the solution permeate through the membrane quickly. The critical size of ion interception of GO membrane with interlayer spacing of 0. 9 nm is 0. 45 nm, which means that GO membrane can be used as a molecular sieve to completely block the ions with hydration radius greater than 0. 45 nm, while the water molecules and hydrated ions with hydration radius less than 0. 45nm can freely penetrate through, thus achieving the separation effect[12,13]. Geim, the discoverer of graphene and winner of the Nobel Prize in Physics, constructed slit-like nanochannels through two-dimensional material micro-nano processing technology to study nanoscale fluid systems.It was found that the graphene structure was formed after removing a certain number of layers in graphite, and the transport velocity of water could reach 1 m/s. These works deepened people's understanding of nanoscale separation performance, and also proposed a new way to control nanoscale fluid systems[14⇓⇓~17]. GO membrane is an ideal membrane separation material because of its unique separation performance, good water permeability and excellent film-forming property. However, there are a large number of oxygen-containing functional groups on the surface and edge of GO, and the GO membrane will swell when immersed in aqueous solution, and the interlayer spacing of GO increases to 1. 35 nm due to the insertion of 2-3 layers of water molecules between GO layers, which affects the ion sieving effect. At the same time, the swelling of the membrane in water also seriously affects its mechanical properties. In the practical application process, GO membrane has some mechanical defects, such as unstable tensile strength, fracture without bearing a certain load, low strength and hardness, which restrict its practical application in the separation fields of solvent dehydration and seawater desalination[18⇓⇓⇓⇓~23].
In order to improve the mechanical properties of GO membranes, some research work has been carried out at home and abroad, through the introduction of active molecules and cations and other particles into the GO membrane layers to form stable bonding, thereby improving the mechanical properties of the membrane. The main methods include the introduction of covalent bonds and non-covalent bonds. Covalent bonds are divided into macromolecular and micromolecular bonds. Non-covalent bonds include hydrogen bonds, ionic bonds and π-π bonds. In this paper, the recent research progress in controlling the mechanical properties of GO membranes is reviewed, and the possible development directions in the future are also prospected.

2 Covalent bond method

There are abundant functional groups on the surface of GO, which can form covalent bonds with some organic or inorganic molecules by chemical crosslinking. The covalent bond has strong bonding strength and can significantly improve the mechanical properties of the GO film. The covalent bond method can be divided into the small molecule covalent bond method and the macromolecule covalent bond method.The crosslinking reaction is shown in Figure 1, Figure 1 (a) is the crosslinking reaction diagram of the macromolecule covalent bond.Through the connection of functional groups,The GO sheets are connected with each other to improve the mechanical properties of the GO composite membrane. Fig. 1 (B) is the crosslinking reaction diagram of covalent bonds of small molecules. The small molecules are connected with functional groups such as carboxyl and hydroxyl on the surface of GO to improve the mechanical properties.

2.1 Small molecule covalent bond method

Gao et al.added small molecules of glutaraldehyde(GA)and water molecules into GO,and intermolecular acetalization reaction took place between GA and the hydroxyl and carboxyl groups on the surface of GO nanosheets to obtain a cross-linked GO composite film.the XRD test results showed that the interlayer spacing changed from the original 0.78 nm to 1.12 nm,the average tensile strength was 101 MPa,and the average Young's modulus was 30.4 GPa,which were greatly improved,being 1.59 and 2.90 times of the original respectively(as shown in Figure 2)[19]。 the mechanical property test And in-situ Raman spectroscopy analysis showed that the increase of tensile modulus and strength of the GA-treated GO films was due to the formation of covalent bonds between GA molecules and adjacent GO nanosheets,and the presence of water molecules could adjust the interlayer spacing and mechanical properties of GO sheets.GA and water were successfully introduced into the interlayers of GO,which effectively improved the interlayer connectivity and thus improved the mechanical strength of GO films,indicating that the introduction of small molecular covalent bonds can effectively improve the mechanical properties of GO films.Hung et al.,Hu et al.,Gong et al respectively found that small molecular compounds such as diamines(ethylenediamine,butanediamine,hexamethylene diamine,etc.)and trimesoyl chloride can form covalent bonds with GO films to improve the mechanical properties of GO films[24⇓~26]。
Some inorganics can also form covalent bonds with GO,and cross-linking them with GO has also been used to improve the mechanical properties of GO films.An et al.Use borate as a cross-linking agent to form a borate-supported lamellar structure between adjacent GO nanosheets[11]。 It can be seen from the XRD test results In Figure 3(a)that the addition of borate changes the interlayer spacing from 0.85 nm to 0.89 nm.the stress-strain curve of the composite membrane is shown in Figure 3(B),which shows that the strength,toughness and ductility of the cross-linked borate GO membrane are improved due to the formation of covalent bonds.in addition,the strengthening effect is different when the content of borate is changed after heat treatment,that is to say,the strengthening effect can be adjusted by adjusting the addition of borate。

2.2 Macromolecular covalent bond method

the use of small molecule crosslinking can improve the strength,while macromolecule crosslinking has a good effect on improving the tensile strength and toughness of GO film.Cheng et al.cross-linked 10,12-pentadien-1-ol(PCDO)with the inner lamellae of the GO membrane,which was similar to building a wall.PCDO was used to build a firm GO wall,and the GO composite membrane was formed through the addition polymerization reaction between functional groups.the toughness of the GO composite membrane was about two times higher than that of the pure GO membrane before compounding,and its tensile strength was also improved,which was due to the formation of covalent bonds with higher cross-linking density between the lamellae[27]。 This result shows that the formation of covalent bonds with macromolecules can simultaneously improve the strength,stiffness and toughness of the GO composite membrane[28⇓⇓⇓⇓⇓⇓⇓~36]。
Cui et al.Crosslinked polydopamine(PDA)with GO membrane and prepared GO/PDA composite membrane by evaporation-induced assembly process.Through the stress-strain curve,it can be found that the tensile strength and toughness of the composite membrane are 1.5 times and 2 times higher than those of the pure GO membrane,respectively,and the composite membrane has good flexibility[37]。 In addition,the tensile strength increased with the increase of the mass fraction of GO,And the maximum value(92.4 MPa)was obtained at 95∶5.This indicates that the introduction of macromolecular covalent bonds by simple chemical modification Can greatly improve the macroscopic mechanical properties of GO materials.Qi et al.and other research groups found that polyethyleneimine(PEI),chitosan,polyacrylamidophenylboronic acid(PAPB),etc.can also form macromolecular covalent bonds with GO sheets to obtain GO-based composite films with enhanced mechanical properties[38⇓⇓⇓~42]。

3 Non-covalent bond method

The introduction of non-covalent bonds, such as hydrogen bonds, ionic bonds and π-π interactions, can also improve the mechanical properties of GO films, but the improvement is relatively weak compared with covalent bonds.

3.1 Ionic bond method

There are a large number of oxygen-containing functional groups on The surface and edge of GO,which makes it easy to exfoliate and functionalize.the GO film is also easy to overcome the van der Waals force or hydrogen bonding in water to separate negative charges.By introducing different metal cations to form ionic bonds between the layers,the mechanical properties can be significantly improved.the crosslinking reaction of this method is shown in Figure 1(C)。
Park et al.Added less than 1 wt%divalent ions to the GO sheet to enhance the mechanical properties of the GO composite film by forming ionic bonds between oxygen-containing functional groups and divalent metal ions[43]。 The results showed that the mechanical properties of the composite membranes modified by Mg2+and Ca2+were significantly improved,and the cyclic loading test showed that the mechanical strength of the composite membranes was increased by 40%~130%.The results of XRD showed that the distance of the composite films modified by Mg2+and Ca2+was increased,which was due to the interaction of metal ions between the GO layers.As shown in Fig.4,after the Ca2+modification,the change of the stress-strain curve in the cyclic loading test,especially the initial part,has a very obvious change,in which red is the first loading,green is the second loading,blue is the third loading,purple is the fourth loading,and navy blue is the fifth loading until fracture.The stress-strain curve of the composite membrane modified by divalent ions increases continuously with the increase of loading and unloading times.In contrast,there was no significant change in the stress-strain curve of the unmodified film at the same number of cycles.The strength of the modified GO membrane is improved compared to the unmodified GO membrane,demonstrating that a small amount(less than 1 wt%)of divalent metal ions can significantly improve the modulus and mechanical properties of the GO membrane 。
Bai et al.Compounded lead ions with GO and prepared a layered large-area flexible GO composite membrane by filtration method.the conductivity of the composite membrane was increased by seven orders of magnitude compared with that of the precursor GO,and the modified GO composite membrane had good flexibility and could be easily bent[44]。 as can be seen from the SEM photograph of the side of the GO-composite film with a thickness of 2.5 microns,the GO-composite film prepared by the method can still maintain a good layered structure,and its mechanical properties are also greatly improved.In addition,some studies have shown that metal ions such As sodium,potassium,lithium and aluminum can also form ionic bonds with GO films,thereby improving their mechanical properties[45⇓⇓⇓⇓~50]。

3.2 Hydrogen Bond Method

hydrogen bonding is also a very important non-covalent bond to improve the mechanical properties of GO membranes.the mechanical properties of GO films can also be greatly improved by hydrogen bonding.the crosslinking reaction diagram of the hydrogen bonding method is shown in Figure 1(d).Medhekar et al.studied the effect of hydrogen bonding on the GO membrane,and they divided the hydrogen bonds in the composite membrane into the following categories:(1)hydrogen bonds between functional groups connected to the same graphene sheet(within the layer)[51]; (2)hydrogen bonds between functional groups attached to adjacent graphene sheets(intermediate layers);(3)Hydrogen bonds in water molecules.Figure 5(a)shows the effect of water content on GO interlayer spacing,where red is the C10O1(OH)1and green is the C10O2(OH)2,representing one and two epoxy and hydroxyl groups per ten carbons,randomly distributed on either side of the datum plane.Fig.5(B)shows the variation of the hydrogen-oxygen bond energy(the interaction energy between two water molecules)with the interlayer distance d,and the optimal distance is 2.5555Åand the intensity is 320 meV.It is shown by inference that water molecules control the common strength of the hydrogen bonding network,which in turn manifests itself in the macroscopic response of these materials.Dry GO films are harder and more brittle than wet ones,and the structure and mechanical properties of GO films can be adjusted by changing the degree of functionalization of individual layers and the water content of the material 。
in addition,Putz et al.compounded GO with hydrophilic material polyvinyl alcohol(PVA)in water and with hydrophobic material polymethyl methacrylate(PMMA)in N,N-dimethylformamide(DMF)solvent.By comparing the cross-linking modification effects of hydrophilic material PVA,hydrophobic material PMMA and GO membrane,it was found that the modulus of GO-PVA nanocomposite membrane prepared with water as solvent was greatly increased compared with that of pure GO membrane,while the modulus of GO-PMMA nanocomposite membrane prepared with DMF as solvent was not increased compared with that of pure GO membrane[52]。 As shown in fig.6,When the GO content is 77.4 wt%,the Young's modulus of the GO-PVA nanocomposite can reach 36.3 GPa,and when the GO content is 80 wt%,the tensile strength reaches 188.9 MPa.the results of the combined experiment,theory and computational simulation show that hydrogen bonding plays an important role in improving the mechanical strength of GO-PVA nanocomposites.During the preparation process,GO is hydrophilic,and there will be a large amount of water between the films.when the water is completely removed,the GO composite film loses all mechanical integrity.DMF is difficult to react with PMMA,which further limits the interaction between PMMA and GO,so the modulus of PMMA based GO film is low.the above test results show that the formation of hydrogen bonds can improve the mechanical properties of GO composite films。

3.3 π-πbond method

In the current research,people are mostly committed to improving the mechanical properties of GO membranes.In the non-covalent modification,besides ionic bonds and hydrogen bonds,there is another important modification method,that is,the formation ofπ-πbonds,which can also enhance the mechanical properties of GO membranes.Zhang et al.compounded polyethylene glycol(PEG)With GO membrane,and enhanced the interaction between PEG and randomly oxidized GO membrane through the interaction between PEG molecules.PEG macromolecules could be easily inserted into the lamellae of GO membrane.with the reaction going on,C O and O—H bonds were broken to form abundantπorbital groups,and thenπ-πbonds were formed between PEG and GO membrane,which improved the mechanical properties of GO membrane[53]。 They proposed a crosslinking effect model based onπ-πbond interaction,as shown In Figure 1(e),which is the crosslinking effect between supercritical polymer and GO membrane mediated byπ-πbond interaction,thus improving the mechanical properties.in the tensile test,the tensile strength of the composite film containing 11.2 wt%polyethylene glycol was 193%higher than that of the pure GO film,and the tensile strength began to decrease when the content of polyethylene glycol exceeded 11.2 wt%.this method of introducingπ-πbonds can improve the hardness and stiffness of GO films,but the preparation of superhard GO materials by This method still needs further exploration and attempt,and the synergistic effect of covalent bonds and non-covalent bonds should be fully exploited。

4 Conclusion and prospect

How to improve the mechanical properties of GO membrane without destroying the layered structure is the key to maintain the high separation performance of GO membrane under long-term operation. It is an effective way to improve the mechanical properties of GO membranes by introducing active molecules or ions between GO sheets to form covalent or non-covalent interactions. The covalent bonds introduced between GO sheets can be divided into macromolecular covalent bonds and micromolecular covalent bonds according to the molecular weight of active molecules or ions. Non-covalent bonds include ionic bonds, hydrogen bonds, and π-π bonds. Covalent bonds have strong interfacial strength, and the strength and hardness of GO membranes can be significantly improved by using small molecule crosslinking, but the toughness is not significantly improved, while the mechanical properties of GO membranes can be comprehensively improved by using long chain macromolecules such as PDA, PEI and PEDO. Non-covalent bonds can also improve the mechanical properties of GO films to some extent, but the effect is not as good as covalent bonds. As shown in Table 1, although some progress has been made in enhancing the mechanical properties of GO film at home and abroad, there is still room for further improvement of its properties, the relevant mechanism is not clear, and how to balance the contradiction between strength and toughness is also an important issue to be studied. Further research work can focus on the following three aspects: (1) Make full use of the rich functional groups on the surface of GO films, and introduce multiple bonding methods at the same time, using the synergistic effect of both, it is expected to further improve the mechanical properties of GO films. For example, macromolecules containing various functional groups can be introduced to form covalent bonds, while divalent cations can be introduced to form ionic bonds; The mechanical properties of the GO separation membrane can also be improved by the synergistic effect of covalent bonds and hydrogen bonds or π-π bonds. (2) The mechanism of different bonding methods to improve the mechanical properties of GO films was explained by theoretical model and theoretical calculation, and the structure-activity relationship was clarified, which provided a theoretical basis for the preparation of high-performance GO films. (3) The existing GO membrane is mainly prepared by vacuum filtration method, which is generally small in size and difficult to prepare on a large scale. The study of continuous preparation method of large area GO membrane is also an important direction to promote its practical application. With the further improvement of performance and the development of large-scale preparation technology, it is expected to realize the practical application of GO membrane in water purification, seawater desalination, ion separation and other fields.

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Funding

the National Natural Science Foundation of China(51572011)

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