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Diamond-Like Carbon Nanofoam from Low-Temperature Hydrothermal Carbonization of a Sucrose/Naphthalene Precursor Solution

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Diamond-Like Carbon Nanofoam from Low-Temperature Hydrothermal Carbonization of a Sucrose/Naphthalene Precursor Solution Journal of C Carbon Research Article Diamond-Like Carbon Nanofoam from Low-Temperature Hydrothermal Carbonization of a Sucrose/Naphthalene Precursor Solution Natalie Frese 1,2, Shelby Taylor Mitchell 2, Amanda Bowers 2, Armin Gölzhäuser 1 and Klaus Sattler 2,* 1 Faculty of Physics, University of Bielefeld, D-33501 Bielefeld, Germany; [email protected] (N.F.); [email protected] (A.G.) 2 Department of Physics and Astronomy, University of Hawaii, 2505 Correa Road, Honolulu, HI 96822, USA; [email protected] (S.T.M.); [email protected] (A.B.) * Correspondence: [email protected]; Tel.: +1-808-856-8941 Received: 7 June 2017; Accepted: 30 June 2017; Published: 6 July 2017 Abstract: Unusual structure of low-density carbon nanofoam, different from the commonly observed micropearl morphology, was obtained by hydrothermal carbonization (HTC) of a sucrose solution where a specific small amount of naphthalene had been added. Helium-ion microscopy (HIM) was used to obtain images of the foam yielding micron-sized, but non-spherical particles as structural units with a smooth foam surface. Raman spectroscopy shows a predominant sp2 peak, which results from the graphitic internal structure. A strong sp3 peak is seen in X-ray photoelectron spectroscopy (XPS). Electrons in XPS are emitted from the near surface region which implies that the graphitic microparticles have a diamond-like foam surface layer. The occurrence of separated sp2 and sp3 regions is uncommon for carbon nanofoams and reveals an interesting bulk-surface structure of the compositional units. Keywords: carbon; nanomaterials; nanofoam; nanostructured; porous; ultralight materials; hydrothermal carbonization 1. Introduction A large variety of nanomaterials can be formed from elemental carbon. Amorphous carbon materials with a high fraction of sp2 bonds are named graphite-like carbons. When sp3 bonds are dominating, the materials are named diamond-like carbons. Their properties depend on the relative abundance of the sp2- and sp3- hybridized carbon atoms [1]. Carbon materials with both graphite- and diamond-like bonds were realized by various synthetic methods, e.g., laser ablation, chemical vapor deposition or hydrothermal carbonization [2]. For example, a material containing graphene sheets and diamond-like structures has been observed after catalytic carbonization of wood charcoal [3]. In this study, we focus on hydrothermal carbonization (HTC) for the synthesis of carbon nanofoam with separated regions of sp2- and sp3-hybridized carbon atoms. Hydrothermal carbonization is a promising method for the synthesis of carbon nanomaterials from biomass [4] for a wide range of applications in fields such as energy storage environment protection [5]. It has been used in industry for the production of fuels and other energetic materials [6]. The carbonization of sucrose biomass usually leads to foam-structured materials consisting of spherical micron-sized particles [7]. It has been shown that a small amount of naphthalene added to a sucrose solution acts as a nucleation seed during the HTC process leading to low density, high-quality carbon foams consisting of micropearls with internal pores [8]. The surface of these materials has been modified by chemical functionalization, and the bulk structure by introducing additional porosity [9]. C 2017, 3, 23; doi:10.3390/c3030023 www.mdpi.com/journal/carbon C 2017, 3, 23 2 of 14 C 2017, 3, 23 2 of 14 Aporosity different [9]. morphology A different morpholo has beengy obtained has been by obtained adding by graphene adding graphene oxide to oxide biomass, to biomass, which which results in carbonresults materialsin carbon materials with higher with degree higher of degree carbonization of carbonization and higher and higher conductivity conductivity [10]. [10]. Porous Porous carbon structurescarbon structures have also have been also producedbeen produced by HTC by HT ofC crude of crude plant plant material, material, which which cancan be up-scaled up-scaled to largeto large quantities quantities with with low low cost, cost, and and these these materialsmaterials may may have have industrial industrial applications applications for forcatalytic catalytic supportsupport andand forfor sorptionsorption purposes [11]. [11]. Other Other pote potentialntial applications applications of ofcarbon carbon nanofoam nanofoam include include hydrogenhydrogen storagestorage [[12],12], cathodes for for batteries batteries [13,14] [13,14 ]or or composites composites for for electrod electrodeses [15,16]. [15,16 It]. follows It follows thatthat the the HTC HTC method method forfor thethe synthesissynthesis ofof functionalfunctional carbon materials materials can can be be used used for for a a broad broad range range of applicationsof applications [2]. [2]. ForFor thisthis study,study, wewe produced carbon carbon nanofo nanofoamam by by naphthalene-assisted naphthalene-assisted hydrothermal hydrothermal carbonizationcarbonization of of sucrose. sucrose. We We find find that that the the amount amount of of added added naphthalene naphthalene critically critically determines determines the the foam morphology.foam morphology. At low At naphthalene low naphthalene concentrations, concentrations, the foam the foam consists consists of an of agglomeration an agglomeration of porous of micropearlsporous micropearls [8]. At higher[8]. At higher concentration, concentration, however, however, the carbonthe carbon nanofoam nanofoam consists consists of of micron-sized micron- irregularlysized irregularly shaped shaped particles particles with sponge-likewith sponge-like surfaces surfaces as visualized as visualized by helium by helium ion microscopyion microscopy (HIM). X-ray(HIM). photoelectron X-ray photoelectron spectroscopy spectroscopy (XPS) reveals (XPS) re a diamond-likeveals a diamond-like carbon carbon surface. surface. The Raman The Raman spectrum spectrum shows the D and G bands of carbon with a distinctly higher G peak. These results shows the D and G bands of carbon with a distinctly higher G peak. These results characterize the characterize the foam as a material consisting of species with a graphite-like core and a diamond-like foam as a material consisting of species with a graphite-like core and a diamond-like shell. The density shell. The density of the analyzed sample is 0.21 g·cm−3, far below the density of graphite, due to of the analyzed sample is 0.21 g·cm−3, far below the density of graphite, due to internal pores. internal pores. 2. Results 2. Results 2.1. Microscopy 2.1. Microscopy Figure1 displays two helium ion microscopy images of the carbon foam sample. Figure1a Figure 1 displays two helium ion microscopy images of the carbon foam sample. Figure 1a shows shows one side of a foam particle. The particle has a diameter of about 200 µm and a uniform rough one side of a foam particle. The particle has a diameter of about 200 µm and a uniform rough surface surface structure. structure. A higher-magnification image of the foam particle is presented in Figure1b. It depicts the upper A higher-magnification image of the foam particle is presented in Figure 1b. It depicts the upper rightright part part of of thethe particleparticle shown in in Figure Figure 1a,1a, and and it it can can be be seen seen that that the the surface surface has has a sponge-like a sponge-like and and frayedfrayed character. character. The The sponge-like sponge-like surfacesurface impliesimplies aa porous foamy structure, which which is is also also indicated indicated by −3 theby lowthe densitylow density of 0.21 of g0.21·cm g·cmof−3the of sample.the sample. The The edge edge resolution resolution of the of imagethe image in Figure in Figure1b is 1b around is 15around nm, which 15 nm, was which determined was determined by the distance by the betweendistance between 25% and 25% 75% and of the 75% maximum of the maximum intensity of aintensity sharp edge of a [ 17sharp]. edge [17]. FigureFigure 1. 1. Helium-ionHelium-ion microscopy images images of of carbon carbon nanofoam, nanofoam, (a) ( ashowing) showing a micron-sized a micron-sized part part of the of the foamfoam and and ((bb)) showingshowing in higher magnification magnification the the sponge-like sponge-like surface surface of ofthe the foam. foam. C 2017, 3, 23 3 of 14 C 2017, 3, 23 3 of 14 2.2. XPS2.2. XPS The chemicalThe chemical composition composition of theof the carbon carbon nanofoam nanofoam surface surface was was determined determined by by XPS.XPS. FigureFigure2 2aa showsshows the C1s the andC1s Figureand Figure2b the 2b O1sthe O1s photoelectron photoelectro signalsn signals of theof the foam foam sample. sample. The The de-convoluted de-convoluted carboncarbon curve curve in Figure in Figure2a consists2a consists of fiveof five peaks, peaks, labeled labeled as as C1–C5.C1–C5. It It has has been been shown shown that that the thesp3- sp3-hybridizedhybridized carbon carbon peak peak is is shifted shifted around around 1 1 eV eV from from the the sp sp2-hybridized2-hybridized carboncarbon peakpeak [[18].18]. Therefore, the twothe maintwo main peaks peaks at 284.4 at 284.4 eV (C1)eV (C1) and and 285.5 285.5 eV eV (C2) (C2) are are assigned assigned to to aromatic aromatic and and aliphatic aliphatic carbons,carbons, respectively.respectively. The The C1 peakC1 peak has has an an area area of of 28%, 28%, whereas whereas thethe C2C2 peak has has an an area area of of 39%. 39%. Since Since XPS XPS is a is a surface-sensitivesurface-sensitive method, method, it itfollows follows that that the thefoam foam surface surface has a hasdiamond-like a diamond-like composition, composition, because becausethe thealiphatic aliphatic carbons carbons dominate dominate in the in spectrum. the spectrum. The remaining The remaining three threepeaks peaks at 286.4 at 286.4eV (19%), eV (19%), 287.3 287.3eV eV (10%) (10%) and and 289.1 eV (4%)(4%) areare assignedassigned toto carbon–oxygencarbon–oxygen bonds;bonds; toto hydroxyl,hydroxyl, carbonylcarbonyl andand carboxylic groups, respectively [19]. Further surface groups such as carboxylic anhydride, lactone or carboxylic groups, respectively [19].
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