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\setlength{\itemindent}{0pt}% \setlength{\parskip}{0pt}% \setlength{\itemsep}{0pt}% \setlength{\parsep}{2pt}% \def\makelabel##1{\upshape ##1}}% } {\end{list}\end{raggedright}} \newenvironment{specHead}[2]% {\vspace{20pt}\hrule\vspace{10pt}% \phantomsection\label{#1}\markright{#2}% \pdfbookmark[2]{#2}{#1}% \hspace{-0.75in}{\bfseries\fontsize{16pt}{18pt}\selectfont#2}% }{} \def\TheFullDate{2014 2014-01-15 (revised: 28 Year 2014 15 January 2014)} \def\TheID{\makeatother } \def\TheDate{2014 2014-01-15} \title{Thermal Stability of Foils Made of Graphene-Oxide and Grapheme -Oxide with Fullerene and their Composites with Methyl Car Boxy Cell u lose and with Beta 1, 3/1, 6 -D-Glucan} \author{}\makeatletter \makeatletter \newcommand*{\cleartoleftpage}{% \clearpage \if@twoside \ifodd\c@page \hbox{}\newpage \if@twocolumn \hbox{}\newpage \fi \fi \fi } \makeatother \makeatletter \thispagestyle{empty} \markright{\@title}\markboth{\@title}{\@author} 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\definecolor{GJBlue}{HTML}{273B81} \definecolor{GJLightBlue}{HTML}{0A9DD9} \definecolor{GJMediumGrey}{HTML}{6D6E70} \definecolor{GJLightGrey}{HTML}{929497} \renewenvironment{abstract}{% \setlength{\parindent}{0pt}\raggedright \textcolor{GJMediumGrey}{\rule{\textwidth}{2pt}} \vskip16pt \textcolor{GJBlue}{\large\bfseries\abstractname\space} }{% \vskip8pt \textcolor{GJMediumGrey}{\rule{\textwidth}{2pt}} \vskip16pt } \usepackage[absolute,overlay]{textpos} \makeatother \usepackage{lineno} \linenumbers \begin{document} \author[1]{ZemanovA Eva} \author[2]{Klouda Karel} \affil[1]{ VAB-Technical University of Ostrava} \renewcommand\Authands{ and } \date{\small \em Received: 9 December 2013 Accepted: 31 December 2013 Published: 15 January 2014} \maketitle \begin{abstract} This contribution contains data on thermal stability of certain materials whose initial precursor is graphite. Graphite was oxidized separately and in a mixture with fullerene C60. The prepared oxides were processed with vacuum filtration to produce foils and their morphology and thermal stability was described. The graphene oxides reacted with nano-cellulose and ß- glucan to produce composites. The prepared composites in the form of foils were tested for thermal stability and further analyzed e.g.by FT-IR, SEM, etc. \end{abstract} \keywords{grapheme oxide, fullerene - c60 Intercalate, composite, nano-cellulose, ß-glucan.} \begin{textblock*}{18cm}(1cm,1cm) % {block width} (coords) \textcolor{GJBlue}{\LARGE Global Journals \LaTeX\ JournalKaleidoscope\texttrademark} \end{textblock*} \begin{textblock*}{18cm}(1.4cm,1.5cm) % {block width} (coords) \textcolor{GJBlue}{\footnotesize \\ Artificial Intelligence formulated this projection for compatibility purposes from the original article published at Global Journals. However, this technology is currently in beta. \emph{Therefore, kindly ignore odd layouts, missed formulae, text, tables, or figures.}} \end{textblock*} \let\tabcellsep& \section[{Introduction}]{Introduction}\par raphite is an allotropic modification of carbon with sp 2 bonds and made up of layers of mutually interconnected hexagonal rings. The layers are arranged in parallel planes 335 pm apart. Carbon atoms in the adjoining layers are not chemically bonded to each other and they are attached by weak van der Waals forces that make it possible for various atoms or molecules in liquid or gaseous form to get in between the carbon layers. The resulting substances are called intercalation compounds of graphite and their characteristic parameter is the so-called "degree of intercalation", which indicates the number of carbon layers between two layers of an inter calated substance \hyperref[b10]{(Klouda, 1985)}.\par Depending on a type of the intercalated substance the graphite plane may be either an acceptor or donor of electrons. Another option is the so-called ?-complex created by intercalation of substances of AX y type, where A is a metal or non-metal with a high Intercalates of graphite with alkali metals have been known since 1930s. They are called intercalates of the first degree with the formula C 8 M (M=K, Rb, Cs), i.e. they are characterized by a stacking sequence of layers of carbon and alkali metal.\par Intercalates of graphite with alkali metals or in combination with other metals have been used in a number of applications as catalysts, e.g. for synthesis of ammonia, synthesis of carbohydrates by hydrogenation of carbon oxides, hydrogenation of olefins, they have sorption properties etc. \hyperref[b10]{(Klouda, 1985)}. Substituents can be chemically bonded to graphite under certain conditions by fluorination or oxidization.\par Fluorination of graphite with elemental fluorine at 400-600°C produces a covalent compound called fluoro graphite CF x , x=0.25-1.12, depending on reaction conditions of the fluorination \hyperref[b10]{(Klouda, 1985)}. Oxidization of graphite with strong oxidizing agents produces grapheme oxide (GO), which is a precursor for chemical preparation of graphene \hyperref[b14]{(Makharza et. al., 2013)}.\par Publications dealing with oxidization of graphite to prepare G-O usually specifya method use das described by specific authors: Hoffmann (HNO 3 , KClO 3 ), Stay dennaier (HNO 3 , KClO 3 ), Tour (P 2 O 5 , KMnO 4 ), Hummers (NaNO 3 , KMnO 4 ). In all those methods the mainchemical agent used is concentrated sulfuric acid (Chang and Pumera, 2013).\par GO is a compound made up of a carbon skeleton with main functional groups, such as carboxyl, carbonyl, epoxy and ether group sandhydroxy-groups. These functional group senable chemical lreactions of GO {\ref (Zang et. al., 2011)} to form covalent bonds with other compounds (e.g.esterification, amidation).\par Another option is a GO reaction to form noncovalent bonds \hyperref[b14]{(Makharza et. al., 2013)}. The possible types of the bonds are hydrogen bonds, van der Waals forces, H-?, cation -?, anion-?, ?-?, electrostatic forces. These non-covalent bonds are employed in preparation of composite polymers, biopolymers {\ref (Yoo, B. M. et. al., 2013)} and in use of GO adsorption and absorption properties \hyperref[b12]{(Kyzas et. al., 2014;}\hyperref[b3]{Fakhri et al., 2013;} engineering, optics \hyperref[b19]{(Russo et. al., 2013)} and biomedicine {\ref (She n et. al., 2012)}.\par Graphene can be prepared by a chemical method which consists in reduction of oxidized carbon (functional groups) in GO with various reducing agents (hydrazine , metal hydride, hydrogen, hydrogen iodide) or reducing methods, such as reflux in a polar solvent, microwaves irradiation, electrochemical reduction \hyperref[b1]{(Dreyer et. al., 2010)}.\par The composition of graphene-oxide and its decomposition by an exothermic creaction in dicates a potential fire risk. This shall apply mainly to industrial production, processing and storage of GO-materials. If stored in a solid form GO shall be protected against sources of heat, electric discharges and exposure to high-intensity light. A question which appeared in publications by Krishnan et al. \hyperref[b11]{(Krishnan et al., 2012)}, i.e. whether GO is afire retarder or fire hazardous material, has defined the objective of this work in which we want to assess behavior of GO and GO-C 60 foils and their composites with cellulose and ß-glucan when thermally exposed. b) Preparation of Graphene-Oxide (GO) and Graphene-Oxide + C 60 (GO-C 60 )\par Graphite was oxidized with a mixture of H?SO?, KMnO? and NaNO? according to Hummers and Offer man {\ref (Hummers and Offer man, 1958)}. Graphite, sulfuric acid and sodium nitrate (for experiments I-II also fullerene C 60 ), were placed into a flask, the mixture was stirred and cooled to 10°C. Potassium permanganate was subsequently added into the reaction mixture through a hopper in small doses. The mixture with the permanganate was slowly heated to 60°C and stirred at that emperature for 3 hours. Then it was left to stand for three days at the laboratory temperature.\par The obtained product was filtered off, washed with big quantity of distilled water until negative reaction to sulfate anions and dried for three days on a Petridish at 50-60°Ctoform foils of GO or GO-C 60 . In order to confirm or to refute our the oretical assumptions about behavior of fullerene in an oxidation mixture we have performed an experiment in which we maintained mutual ratios of carbon to the other reagents as those used in the experiment with graphite (0.7g C 60 , 1 g NaNO 3 , 2 g KMnO 4 , 18 ml H 2 SO 4 ). Also there action times and subsequent treatment were equivalent. After vacuum filtration we did not obtain foils but after the drying we obtained black loose powder (hereinafterC 60oxi). The powder was investigated with FT-IR, TGA, DSC analysis and the results were compared with analyses of the initial fullerene. d) Reaction of GO and GO-C 60 Foils with Cellulose in Acid Environment GO (0.3 g) and GO-C 60 (0.3 g) foils were placed into Erlenmeyer flasks and 10 ml of distilled water was added. Foil schanged into suspension safter 3 day so firregularstirring and short-termultrasonification. Subsequently, cellulose was added into the flasks (0.65 g) and 8 ml H 2 SO 4 (96\%). The reaction was exothermic. The mixture was ultrasonificated in a water bath at 40°C. Then the flask content was poured into 50 ml of distilled water and neutralized with a solution of sodium hydro carbonate (NaHCO 3 ) until neutral reaction. The product was then vacuum filtered and washed on a filter with ca. 40 ml of distilled water, dried at 50°C on a Petri dish on which it formed foils. e) Reaction of GO with ß-Glucan Graphene oxide (prepared according to \hyperref[b5]{Hummers, 1958)} ii. Employed methods Ultrasonification with PS4000A, power output 500W, thermostat 0-77°C, frequency 35 kHz ATR analysis by means of FTIR spectrometry was performed using the spectrometer Brucker Aplha/FT-IR, ART crystal (identified as Platinum Diamond 1 Ref1), software OPUS 6, 5, source IR SiC Globar. The number of spectrum scans was 24, resolution 4 cm-1 , spectrumrange 375-4000 cm-1 .\par Thermal analyses TGA and DSC of the prepared an of ibers were performed on STA 1500, Instrument Specialists Incorporated-THASS, analytical scale SUMMIT, SI 234-4, at flowrate 20 ml/min., heatingrate 10°C/min., ceramiccrucible, diameter 5 mm and height 8 mm, degradation medium: air.\par Morphology of then an of ibers was determined with SEM Phenom FEI and SEM FEI Quanta 650 FEG (USA).\par into Erlenmeyer flasks with 25 ml of distilled water. No suspension was formed after 48 hours and it was necessary to performer peated ultrasonification 5x 2 minutes to prepare the suspension. Beta -glucan (0.45 g) was added into the suspensions and in one of the flasks also 0.7 ml of concentrated H 2 SO 4 (an exothermic process occurred after the acid was added).\par i. Visualization of the flask content\par ? without H 2 SO 4 gel (product I)\par ? with H 2 SO 4 suspe nsion(product II) Subsequently, Erlenmeyer flasks were placed into a water bath (40°C) and ultrasonificated 3 times for 2 minutes. Then they were left to stand for 15 day sat the laboratory temperature. The flask with the product I (GO-ßG) was vacuum filtered and the resulting black foil was dried at 50-55°C. The flask with the product II (GO-ß G, H+) was poured into a 300 ml flask, diluted with 200 ml of distilled H2O and subsequently 12 times decanted top H 6.5. The flask contained brown spongycoagu late in1/3 of the flask volume. A part of the coagulate was vacuum filtered and it formed a brown foil which was dried at 50-55°C. \section[{II.}]{II.} \section[{Results}]{Results} \section[{a) Oxidation of Graphite and Mixture of Graphite-C 60}]{a) Oxidation of Graphite and Mixture of Graphite-C 60}\par The foil sobtained by vacuum filtration from the product of oxidation of graphite alone and the product of joint oxidation with C 60 had clearly different morphologies (see Fig. {\ref 1}). GO-C 60 foils looked more compact than GO foils. When inspecting the morphology with electron micros copy the GO-C 60 foil has a rougher surface (see Fig. {\ref 2}). For GO-C 60 foils we also determined its texture. The specific surface of the foil samples GO-C 60 was and the volume of adsorbed monomolecular layer was 5.03 ml/g. The volume of me so pores or macro pores was 0.286 ml/gin comparison with the volume of micro pores which was0.001 ml/g. The volume representation of me so pores was ca. 286 times higher than that of micro pores. The sample had a me spoor us character with some representation of macro pores. The sample contained very little micro pores (see the volume representation -only0.001 clogged. Theme sopores included the following fractions: 1.5-3 nm (ca. 38\%), 3-5 nm (ca. 13\%) and 5-10 nm (ca.5\%) and 10-50 nm (ca.8\%). As for macro pores, the sample contained only one fraction, while ca. 24\% of the specific surface was formed by macro pores with the diameter 50-200 nm. The measured parameters are shown in Table {\ref No} Subsequently, the foils were examined with X-ray analysis (Fig. \hyperref[fig_2]{3}), FT-IR, TGA and DSC analyses. The X-ray analysis has proved a negligible difference in expansion of the space between the layers, see Fig. When preparing GO by oxidation methods FT-IR is usually indicated as a method for identification of the basic functional groups. In most cases the authors indicate vibration ranges for the given groups: 3000 -3700 cm-1 ? (-COOH, -OH, H2O) 1850 -1750 cm-1 ? (-C=O) 1650 -1750 cm-1 ? (car boxy COOH) 1500 -1600 cm-1 ? (sp2 C=C) 1280 -1320 cm-1 ? (epoxides C-O-C) At the same time, ranges that follow may contain the following vibrations: 1280 -1500 cm-1 : ethers, epoxides, ketones, peroxides, benzoquinone 1100 -1280 cm-1 : peroxides, ethers, ketones, lactones, anhydrides, epoxides, benzoquinones 900 -1100 cm-1 : lactones, peroxides, hydroxyls, 1, 3 dioxane, anhydrides, epoxides, car boxy les-OH bond vibration at 3420 cm-1 , C=O bond vibrationat1720 -1740 cm-1 .\par The mutual comparison of spectrums we obtained for GO and GO-C 60 is shown in Fig. {\ref 4} The difference between the GO and GO-C60spectrums is in the ratio of the mutual adsorbances for the vibrations: GO 1390 1274 1228 cm-1 GO-C 60 1378 1278 1228 cm-1 In thespectrumrange700 -450 cm-1 the ads or bance of GO has a medium value while for GO-C 60 it is high; in general, GO-C 60 demonstrates higher adsorbances throughout the entire spectrum range. c) Thermal Tests of GO and GO-C 60 foils Two prominent peaks were detected for samples of GO and GO-C 60 foil son the DSC curve (Fig. {\ref 5}) which corresponded to exothermic processes. The first exothermic process was accompanied by a substantial drop of weight: for go by 43.6\% and for GO-C 60 it was even higher-51.1\% (see Tab. 2).\par In the case of GO the first exothermic process occurred at 190.9°Cwith the maximum at 225°C and thermal effect of 508.4 kJ/kg; in the case of GO-C 60 the process started earlier, at 182.6°Cwith the maximum at 205°Cand the thermal effect was lower than for GO. The values of thermal effects in the individual temperature intervals are provided in Tab.3.The second exothermic effect in the case of GO has its maximum at 450°C, while for GO-C 60 it was already at 390°C and the detailed shape of the curve was different (compare Figures5 and 6). For GO-C 60 the weight loss during the second exothermic effect was lower than during the exothermic effect in the case of GO, which means a situation different from the first effect.\par The weight losses until the first exothermic process are essentially the same for both the foils (ca. 20\%) with mild end other mic effects, with a higher thermal effect for GO (anticipated dehydration). Also the overall thermal effect of decomposition is higher for GO-C 60 foil by ca. 30\% (see Tab.3). When performing the experiments we had some expectations about the course and results of there action. The functional groups expected on GO were the following: carboxyl, carbonyl, epoxide, hydroxyl and partly also lactone or sulfonic group. Fullerene C?? was expected to have the following groups on its molecule: -SO?H, -OH, -NO?, -ONO?, epoxide group. Covalent bonds may form between those groups (esterification, dehydration, addition),as well as noncovalent ones -hydrogen bonds, ?-? interaction, vander Waals forces. Also intercalation of a fullerene molecule may occur in the graphene-oxide space. Even breakage of a fullerene molecule in the conditions of oxidation cannot be excluded. One quoted work (Trzaskowki et al., 2013) deals with energy options of a combination of graphene with C 60 on the condition that graphene surfaceis either defect-free or with defects. Chemical attachment of C 60 on amonolayer of graphene is not possible for energy reasons. However, in presence of various defects on the grapheme C-layer, such as e.g. formation of 4-and 5-atomic rings, Stone-Wales defect and other types of defects (e.g. flower defect, octa-penta-, heptadisrupted cyclic formations) may provide spaceorre active points for potential bonds with fullerene C 60 .\par One of the defects mentioned for the graphene structure is the so-called "adatom"-an adsorbed atom. It is a defect in which e.g. transition metal is adsorbedon the C lattice. Adsorption of transition metals changes physicochemical properties and biocompatibility of graphene or GO \hyperref[b4]{(Faye, 2012}; Ne to, 2009). We have identified a similar defect in the prepared GO: it was e.g. an atom of Fe identified by EDAX in the GO structure (Fig. \hyperref[fig_5]{7}). We performed the so-called blank test to get some notion of how fullerene behaves in the oxidizing environment to which it is exposed jointly with graphite. \section[{d) FT-IR Analysis of C 60 -Oxi and Initial C 60}]{d) FT-IR Analysis of C 60 -Oxi and Initial C 60}\par The measured IR spectrum of the initial fullerene C 60 is provided in Fig. {\ref 8}. The main characteristic vibrations for C 60 \hyperref[b34]{(Saeedfar et al., 2013)} are 522 cm-1 , 573 cm-1 , 1159 cm-1 , and 1426 cm-1 and they are also a part of the C 60 -oxi spectrum.\par For C 60 -oxi (Fig. {\ref 9}) we have identified an additional weak vibration in the absorption interval 1556-1644 cm-1 (probably C=C, C=O), 1000-1100 cm-1 (probably C-O-C epoxy, alkoxy, C-CO-C) and a medium vibrationat 702 cm-1 (probably a substituted romatic ring). Based on characteristic vibrations of functional groups we can probably exclude presence of the following functional groups on the C 60 -oxi molecule:-OH, -COOH, -COOR, -SO 3 H, -NO x . In the measure demperature range, as indicated by the TGA and DSC curves (Fig. {\ref 10-11}) up to ca. 420°C,there were no thermal effects on either of the tested sample sand the weight loss of both the samples was comparable in units of percents (6.1\% for C 60 and 8.6\%for C 60 -oxi). In the temperature range of 420-600°C both the samples underwent exother micreactions, however the thermal effects were very different. The thermal effect of C 60 -oxi was 20 times higher than that of the initial C 60 (1947 kJ/kgfor C 60 -oxi and 180 kJ/kg for C 60 ). The weight loss of C 60 -oxi (56.7\%) was twice bigger than that of C 60 (28.8\% ). The resistance of C 60 -oxi against thermal exposure was partly disrupted. We anticipate partial oxidation of the C-skeleton (IR-spectrum Fig. {\ref 9}) and thus disruption of its consistence (electron balance) which means that defects can appear in the carbon structure when the material is heated -e.g. the Stone-Wales defect (Kabiretal., 2011). \section[{Global Journal of Researches in}]{Global Journal of Researches in} \section[{Global Journal of Researches in Engineering}]{Global Journal of Researches in Engineering}\par We have identified a similar reduction of resistance of the fullerene carbon skeletoninits bromoderivative. After end other micdisruption of C-Brbond the C 60 moleculefully (100\%) decomposed at 420-550°C.\par We are fully aware of the fact that this so-called" blind test" may not completely correspond to the oxidation process in presence of graphite or grapheneoxidein which a carbo-catalytic effect may apply (H 2 SO 4 HCl), ratio of cellulose and acid, time of hydrolysis and on reaction temperature. Naturally, the result is also influenced by the type of the initial cellulose which can come from hard or soft wood, bamboo, sisal, cotton etc. All those factors in fluenceyield and size of the prepared cellulose nano fibers (Ioelovich, 2012; Li and Rage uskas, 2011). The prepared nano crystalline cellulose can bechemically modified, e.g. esterifed, carboxy lated oroxidized \hyperref[b16]{(Peng et al., 2011)}. It may be also used asa composite inpolymersor as a matrix for metal nano particles.\par In our case we performed hydrolysis of methyl car boxy cellulose in presence of suspensions of GO and GO-C 60 . We assumed that mutual interconnection may occur by a chemical reaction (e.g esterification, interconnection with C-O-C bond etc.) or physic chemical bond (e.g. hydrogenbonds). The foils prepared by vacuum filtration of the reaction product were subject to microscopic surface analysis, FT-IR, TGA and DSC analysis.\par Morphology of the surfaces as shown by microscopic analysis (see Fig. \hyperref[fig_0]{12}) was different and it suggesteda potential method of interconnection between GO / GO-C 60 and nanocellulose. The detailed morphology (electron microscope) of the prepared composite foils is shown in Fig. \hyperref[fig_2]{13} We assume that in the first case the cellulose hydrolysis was only partial and whiskers of nano cellulose generated after the hydrolysis were of bigger size. At the same time, there was no reaction of C=O groups, unlike in the case of GO, where IR analysis of the product of reaction with cellulose identified no vibration at 1722 cm-1 ,which was present in the spectrum of the original GO. The other vibrations characterizing the groups C-O, C=C, C-O and C-O-C shifted their frequencies and also the mutual absorption ratios were different (Fig. \hyperref[fig_10]{15}).\par The same applies in respect to the initial GO, GO-C 60 and cellulose (compare with the spectrums in Fig. {\ref 4} For the new products in both cases the IR spectrums did not contain the peaksat1278 cm-1 (1274 cm-1 ) and 1228 cm-1 which in the original spectrums GO-C 60 and GO had the assigned vibrations of epoxy groups.\par Similar results, i.e. demonstration of deoxidizing (reduction) process, were described for the mutual reaction of GO with heparin TGA curves of samples (see Fig. \hyperref[fig_12]{16}) of composites can be divided into several sections with different slopes, i.e. different weight loss rates. This division, including corresponding temperature intervals and corresponding weight losses, is shown in Tables \hyperref[tab_5]{4 and 5}, which provide parameters of the detected thermal processes on the DSC curve.\par For composite samples the DSC curve showed one peak corresponding to an endothermic process and two peaks corresponding to exothermic processes. The second exothermic process was very substantial in both the samples. For the GO-C 60 -cellulose sample the exothermic process started at 319.8°C and the peak area on the DSC curve was 3379.2 kJ/kg. Equally significant exothermic process in the GO-cellulose sample started at 341.5°C and the peak area on the DSC curve was 5261. The comparison of thermal stabilities of the prepared GO and GO-C60composites with cellulose indicates that the foil prepared from GO is thermally more stable but its decomposition releases more thermal energy.\par A principle difference can be found when we compare thermal stability (weight loss) of the initial foils of GO and GO-C 60 and thermal stability of their composites with cellulose. The weight loss in the temperature interval 25-220°C was 63\% for GO foil sand 72\% for GO-C 60 foils. For the composites the weight loss was 32\% and 22\% respectively, which means a major difference. A completely different is the thermal decomposition of the initial cellulose. The decomposition in the temperature interval 25-154 o C is accompanied by an endothermic process with the thermal effect 3053.7 kJ/kg and the weight loss of the sample is 64\%. i) GO Reaction with ß-1,3-1,6-D-Glucan Glucans rank among homopolymsacharides, they have a long chain with only one structural component-glucose (hexose). Glucose in the chain is attached in the positions 1,3 and 1,6. Smaller chains branch off from the main chain. The structure of glucans is of extraordinary importance inactivation of the immunity system where branching of the side chains plays a majorrole. ß-D-glucans are indigestible polysaccharides that occur in nature in sources such as cereal grains, yeasts, fungi, bacteria and algae. Biological effects of beta-glucans are manifested at several levels. The main role consists in activation of immunity system cells (macrophage) and they also performanti-carcinogenic, antimicrobial, antiviral and antialergic activities. Betaglucans also have a radio protective effect-they deactivate free radicals \hyperref[b8]{(Chovancová and ?turdík, 2005)}.\par We performed reaction of beta-glucan with graphene-oxide under ultrasonification conditions with out sulfuric acid and in acid environment. j) FT-IR Analysis of the Foils (GO-ßG and GO-ßGH+)\par The obtained spectrums of the products are shown in Fig. \hyperref[fig_5]{17from} left to right: GO-ßG, GO-ßGH+ and initial ßG. In the last picture d) the three spectrums are compared. The values of the initial GO are: C-O-C 1068 cm 1 , 9.79 cm-1 , -OH 3149-3186 cm-1 , -C=C-1613 cm-1 . k) Thermal Stability of the Product (GO-ßG, GO-ßGH+) and Initial ßG \section[{Global}]{Global}\par The measured results in a graphic form are provided in Fig. {\ref 18}-20 and interpretation of the TGA and DSC curves is provided in Tables \hyperref[tab_7]{6-7}.The DSC curve of ßG features one peak corresponding to an end other micthermal process with minimum weight loss and prominent, partly overlapping peaks that correspond to exothermic thermal processes which start at 257°C and are accompanied by a significant loss of the sample weight.\par A common characteristic of both the prepared composite products is that their weight loss curves (TGA)can be approximated with a line -continuous linear reduction of weight, unlike the step weight loss in case of ßG which was up to 70\% (see Fig. {\ref 18}) and in case of GO up to 60\% (see Fig. {\ref 5}). The products differ from each other by the number of exothermic effect sand the shift of the last exothermic effect by 42°C in favor of GO-ß G H+.\par The overall thermal effect in the course of decomposition decreases from the initial ßG to the GO-ßGH+ composite (see Tab. \section[{Conclusion}]{Conclusion}\par Joint oxidation of graphite and fullerene C 60 in the ratio2:1makes it possible to prepare a compound din form of compact foils but it has a lower thermal stability and its thermal decomposition is accompanied by thermal effects that are 30\% bigger than effects produced by foils without fullerene. A method of attachment between oxidized graphite and fullerene has not been demonstrated. The prepared foil can also have other chemical and physicochemical properties thanks to the fullerene molecule {\ref (Trosh in et al., 2008)}.\par Thermal decomposition of composites of GO andGO-C 60 with nano cellulose is accompanied by bigger thermal effects than the effects produced by the initial GO andGOC 60 foils. The same applies also for ßglucan in respect to GO. However, the thermal effect of the decomposition is lower than for ß-glucan alone.\par The products we prepared were in the form of foils (membranes), with the exception of the "blank test" of fullerene oxidation. GO-foils (papers) are prepared by vacuum filtration of GO dispersion. This is the basic method of its preparation which we have also applied. We are fully aware of the fact that mechanical, electronic, chemical and biological properties and the related toxicological properties are affected by many factors which may have influenced our results of thermal stability measurements. The first factor is the method of GO preparation and thus there sultingratio of C/O and topology of the C-skeleton (its defects).The composition of the liquid phase and the concentration (Park et al., 2012) of the filtered suspension influence the foil thickness, as well as the filtration rate, and if the suspension is ultrasonificated then also its duration, temperature and power of the device play a role \hyperref[b26]{(Liao et al., 2011)}. Properties of foils are also influenced by some specific treatments, such as washing of foils with solution of MCl 2 (Ca, Ba, Mg), while the carbon layers are connected in a plane, across via dialdehyde \hyperref[b31]{(Hu et al., 2011)}, or its impregnatione.g. with Ti, Ag, Cu \begin{figure}[htbp] \noindent\textbf{12}\includegraphics[]{image-2.png} \caption{\label{fig_0}Figure 1 :Figure 2 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-3.png} \caption{\label{fig_1}}\end{figure} \begin{figure}[htbp] \noindent\textbf{3}\includegraphics[]{image-4.png} \caption{\label{fig_2}Figure 3 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-5.png} \caption{\label{fig_3}}\end{figure} \begin{figure}[htbp] \noindent\textbf{56}\includegraphics[]{image-6.png} \caption{\label{fig_4}Figure 5 :Figure 6 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{7}\includegraphics[]{image-7.png} \caption{\label{fig_5}Figure 7 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{89}\includegraphics[]{image-8.png} \caption{\label{fig_6}Figure 8 :Figure 9 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{1011}\includegraphics[]{image-9.png} \caption{\label{fig_7}(Figure 10 :Figure 11 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-10.png} \caption{\label{fig_8}(}\end{figure} \begin{figure}[htbp] \noindent\textbf{1213}\includegraphics[]{image-11.png} \caption{\label{fig_9}Figure 12 :Figure 13 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{15}\includegraphics[]{image-12.png} \caption{\label{fig_10}Figure 15 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-13.png} \caption{\label{fig_11}}\end{figure} \begin{figure}[htbp] \noindent\textbf{16}\includegraphics[]{image-14.png} \caption{\label{fig_12}Figure 16 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-15.png} \caption{\label{fig_13}}\end{figure} \begin{figure}[htbp] \noindent\textbf{181920}\includegraphics[]{image-16.png} \caption{\label{fig_14}HFigure 18 :Figure 19 :Figure 20 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-17.png} \caption{\label{fig_15}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-18.png} \caption{\label{figure18}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-19.png} \caption{\label{figure19}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-20.png} \caption{\label{figure20}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-21.png} \caption{\label{figure21}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-22.png} \caption{\label{figure22}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-23.png} \caption{\label{figure23}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-24.png} \caption{\label{figure24}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-25.png} \caption{\label{figure25}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-26.png} \caption{\label{figure26}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-27.png} \caption{\label{figure27}}\end{figure} \begin{figure}[htbp] \noindent\textbf{}\includegraphics[]{image-28.png} \caption{\label{figure28}}\end{figure} \begin{figure}[htbp] \noindent\textbf{2} \par \begin{longtable}{P{0.09377224199288256\textwidth}P{0.0786476868327402\textwidth}P{0.49608540925266903\textwidth}P{0.18149466192170818\textwidth}} Sample No.\tabcellsep Interval No.\tabcellsep Temperature range (°C)\tabcellsep Weight loss (\%)\\ \tabcellsep 1\tabcellsep 25.0 -142.4\tabcellsep 11.0\\ \tabcellsep 2\tabcellsep 142.4 -213.5\tabcellsep 8.8\\ GO foils\tabcellsep 3 4\tabcellsep 213.5 -222.3 222.3 -368.8\tabcellsep 43.6 2.8\\ \tabcellsep 5\tabcellsep 368.8 -473.0\tabcellsep 18.1\\ \tabcellsep 6\tabcellsep 473.0 -600.0\tabcellsep 6.1\\ \tabcellsep 1\tabcellsep 25.0 -87.1\tabcellsep 4.4\\ \tabcellsep 2\tabcellsep 87.1 -153.0\tabcellsep 8.2\\ GO-C 60 foils\tabcellsep 3 4\tabcellsep 153.0 -197.0 197.0 -205.0\tabcellsep 8.0 51.1\\ \tabcellsep 5\tabcellsep 205.0 -281.3\tabcellsep 10.8\\ \tabcellsep 6\tabcellsep 281.3 -490.9\tabcellsep 18.0\end{longtable} \par \caption{\label{tab_2}Table 2 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{3} \par \begin{longtable}{P{0.10252918287937743\textwidth}P{0.08268482490272373\textwidth}P{0.3042801556420233\textwidth}P{0.16536964980544747\textwidth}P{0.10914396887159532\textwidth}P{0.08599221789883268\textwidth}} Sample No.\tabcellsep Thermal process No.\tabcellsep Temperature range (°C)\tabcellsep Î?"H (kJ/kg) *\tabcellsep H f1 (mW)\tabcellsep ?Î?"H (kj/kg)\\ \tabcellsep 1\tabcellsep 25.0 -154.1\tabcellsep 874.6\tabcellsep 15.8\tabcellsep \\ GO foils\tabcellsep 2\tabcellsep 190.9 -241.1\tabcellsep -508.4\tabcellsep 107.4\tabcellsep -910.6\\ \tabcellsep 3\tabcellsep 356.5 -492.1\tabcellsep -1277.1\tabcellsep 31.0\tabcellsep \\ \tabcellsep 1\tabcellsep 42.0 -124.2\tabcellsep 141.7\tabcellsep 6.4\tabcellsep \\ GO-C 60 foils\tabcellsep 2\tabcellsep 182.6 -221.5\tabcellsep -308.7\tabcellsep 71.1\tabcellsep -1204.1\\ \tabcellsep 3\tabcellsep 319.7 -481.6\tabcellsep -1037.1\tabcellsep 28.1\tabcellsep \end{longtable} \par {\small\itshape [Note: *Î?"H = thermal effect of the process based on the DSC curves (Î?"H > 0?endothermic process, Î?"H < 0?exothermic process) Global Journal of Researches in Engineering ( ) Volume XIV Issue I Version I Year 2014]} \caption{\label{tab_3}Table 3 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{4} \par \begin{longtable}{P{0.08900523560209424\textwidth}P{0.06897905759162304\textwidth}P{0.5117801047120419\textwidth}P{0.18023560209424083\textwidth}} Sample No.\tabcellsep Interval No.\tabcellsep Temperature range (°C)\tabcellsep Weight loss (\%)\\ \tabcellsep 1\tabcellsep 25.0 -42.4\tabcellsep 0.3\\ \tabcellsep 2\tabcellsep 42.4 -123.9\tabcellsep 6.9\\ GO-C 60 -cel.\tabcellsep 3 4\tabcellsep 123.9 -168.9 168.9 -347.8\tabcellsep 11.9 18.5\\ \tabcellsep 5\tabcellsep 347.8 -474.3\tabcellsep 36.4\\ \tabcellsep 6\tabcellsep 474.3 -600.0\tabcellsep 6.8\\ \tabcellsep 1\tabcellsep 25.0 -57.3\tabcellsep 0.9\\ \tabcellsep 2\tabcellsep 57.3 -120.8\tabcellsep 10.1\\ \tabcellsep 3\tabcellsep 120.8 -144.6\tabcellsep 3.0\\ GO -cel.\tabcellsep 4\tabcellsep 144.6 -180.6\tabcellsep 13.2\\ \tabcellsep 5\tabcellsep 180.6 -396.5\tabcellsep 20.6\\ \tabcellsep 6\tabcellsep 396.5 -522.6\tabcellsep 48.3\\ \tabcellsep 7\tabcellsep 522.6 -545.0\tabcellsep 2.5\\ \tabcellsep 1\tabcellsep 25.0 -62.9\tabcellsep 8.5\\ \tabcellsep 2\tabcellsep 62.9 -124.9\tabcellsep 55.6\\ cellulose\tabcellsep 3\tabcellsep 124.9 -265.8\tabcellsep 3.3\\ \tabcellsep 4\tabcellsep 265.8 -333.4\tabcellsep 15.8\\ \tabcellsep 5\tabcellsep 333.4 -600.0\tabcellsep 10.5\end{longtable} \par \caption{\label{tab_4}Table 4 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{5} \par \begin{longtable}{P{0.29078947368421054\textwidth}P{0.05219298245614035\textwidth}P{0.23859649122807017\textwidth}P{0.124890350877193\textwidth}P{0.08015350877192982\textwidth}P{0.06337719298245613\textwidth}} Sample No.\tabcellsep Thermal process No.\tabcellsep Temperature range (°C)\tabcellsep Î?"H (kJ/kg) *\tabcellsep H f1 (mW)\tabcellsep ?Î?"H (kj/kg)\\ \tabcellsep 1\tabcellsep 31.6 -115.3\tabcellsep 159.9\tabcellsep 5.7\tabcellsep \\ GO-C 60 -cel.\tabcellsep 2\tabcellsep 115.3 -187.2\tabcellsep -251.1\tabcellsep 18.7\tabcellsep -3470.2\\ \tabcellsep 3\tabcellsep 319.8 -531.0\tabcellsep -3379.0\tabcellsep 59.2\tabcellsep \\ \tabcellsep 1\tabcellsep 25.0 -133.1\tabcellsep 757.5\tabcellsep 17.7\tabcellsep \\ GO -cel.\tabcellsep 2\tabcellsep 133.1 -208.1\tabcellsep -581.2\tabcellsep 41.7\tabcellsep -5085.1\\ \tabcellsep 3\tabcellsep 341.54 -557.2\tabcellsep -5261.4\tabcellsep 76.8\tabcellsep \\ \tabcellsep 1\tabcellsep 25.0 -154.0\tabcellsep 3053.7\tabcellsep 86.2\tabcellsep \\ cellulose\tabcellsep 2\tabcellsep 247.9 -344.8\tabcellsep -211.3\tabcellsep 12.2\tabcellsep +2805.7\\ \tabcellsep 3\tabcellsep 372.0 -414.6\tabcellsep -36.7\tabcellsep 2.3\tabcellsep \\ \multicolumn{3}{l}{*Î?"H = thermal effect of the process based on DSC curves}\tabcellsep \tabcellsep \tabcellsep \\ \multicolumn{3}{l}{(Î?"H > 0?endothermic process, Î?"H < 0?exothermic process)}\tabcellsep \tabcellsep \tabcellsep \end{longtable} \par \caption{\label{tab_5}Table 5 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{6} \par \begin{longtable}{P{0.056068601583113456\textwidth}P{0.07176781002638521\textwidth}P{0.53377308707124\textwidth}P{0.1883905013192612\textwidth}} Sample No.\tabcellsep IntervalNo.\tabcellsep Temperature range (°C)\tabcellsep Weight loss(\%)\\ \tabcellsep 1\tabcellsep 25.0 -114.4\tabcellsep 5.5\\ \tabcellsep 2\tabcellsep 114.4 -278.1\tabcellsep 8.6\\ ßG\tabcellsep 3 4\tabcellsep 278.1 -330.3 330.3 -412.7\tabcellsep 52.2 17.0\\ \tabcellsep 5\tabcellsep 412.7 -462.4\tabcellsep 14.8\\ \tabcellsep 6\tabcellsep 462.4 -475.9\tabcellsep 14.8\\ \tabcellsep 1\tabcellsep 25.0 -149.4\tabcellsep 9.9\\ \tabcellsep 2\tabcellsep 149.4 -225.5\tabcellsep 12.3\\ GO-ßG\tabcellsep 3 4\tabcellsep 225.5 -292.3 292.3 -337.9\tabcellsep 4.7 26.7\\ \tabcellsep 5\tabcellsep 337.9 -438.4\tabcellsep 15.7\\ \tabcellsep 6\tabcellsep 438.4 -529.8\tabcellsep 30.7\\ \tabcellsep 1\tabcellsep 25.0 -124.2\tabcellsep 9.9\\ \tabcellsep 2\tabcellsep 124.2 -204.2\tabcellsep 4.2\\ GO-ßGH +\tabcellsep 3 4\tabcellsep 204.2 -230.8 230.8 -321.6\tabcellsep 10.9 22.5\\ \tabcellsep 5\tabcellsep 321.6 -480.9\tabcellsep 25.9\\ \tabcellsep 6\tabcellsep 480.9 -550.2\tabcellsep 26.9\end{longtable} \par {\small\itshape [Note: X-the indicated intersections of tangents to the respective bends of the TGA curve]} \caption{\label{tab_6}Table 6 :}\end{figure} \begin{figure}[htbp] \noindent\textbf{7} \par \begin{longtable}{P{0.06419939577039274\textwidth}P{0.07447129909365559\textwidth}P{0.33126888217522654\textwidth}P{0.177190332326284\textwidth}P{0.11555891238670694\textwidth}P{0.08731117824773414\textwidth}} Sample No.\tabcellsep Thermal processNo.\tabcellsep Temperature range (°C)\tabcellsep Î?"H (kJ/kg) *\tabcellsep H f1 (mW)\tabcellsep ?Î?"H (kj/kg)\\ ßG\tabcellsep 1 2\tabcellsep 25.0 -153.9 257.5 -528.4\tabcellsep 805.9 -4392.5\tabcellsep 21.3 81.0\tabcellsep -3586.6\\ \tabcellsep 1\tabcellsep 25.0 -157.0\tabcellsep 825.3\tabcellsep 16.9\tabcellsep \\ GO-ßG\tabcellsep 2 3\tabcellsep 157.0 -228.8 311.0 -356.5\tabcellsep -147.1 -36.3\tabcellsep 8.9 6.2\tabcellsep -2734.9\\ \tabcellsep 4\tabcellsep 383.3 -539.3\tabcellsep -3376.8\tabcellsep 66.4\tabcellsep \\ \tabcellsep 1\tabcellsep 25.0 -145.9\tabcellsep 685.2\tabcellsep 16.7\tabcellsep \\ GO-ßGH +\tabcellsep 2\tabcellsep 197.2 -250.0\tabcellsep -313.5\tabcellsep 38.2\tabcellsep -2084.7\\ \tabcellsep 3\tabcellsep 425.4 -589.3\tabcellsep -2456.4\tabcellsep 46.2\tabcellsep \end{longtable} \par \caption{\label{tab_7}Table 7 :}\end{figure} \footnote{© 2014 Global Journals Inc. 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