Spectral analysis, thermal behavior, XRD and morphology study in synthesis of carbon nanotubes decorated by Cysteamine
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A simple and efficient procedure for synthesis of Thiolic Composite with use Oxide Multi Walled Carbon Nanotube
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A simple and efficient procedure for synthesis of composite thiol with use oxide multi walled carbon nanotube and sulfur
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Behnam Maazinejad, Hamidreza Sadegh, Imran Ali, Ramin Shahryari Ghoshekandi, Vahid Ali
 
 
Abstract
In this paper, the effects of multi-Walled carbon nanotubes (MWCNTs) were studied as supports for the synthesis of MWCNT-COOH-Cysteamine nanocomposite. At first Purification MWCNT in H2SO4 and HNO3, solved and the solution earned ultrasound was to attain the equilibrium temperature to functionalization of carboxylate multi walled carbon nanotubes (MWCNT-COOH). Then using Cysteamine hydrochloride and NHS and DMF and EDC and MWCNT-COOH the mixture was refluxing. The prepared on thiol derivatized nanocomposite were analyzed by X-ray Diffraction, Scanning electron microscope, FTIR spectroscopy, Transmission Electron Microscopes (TEM) and Thermogravimetric Analysis (TGA).
Keywords
MWCNTs, Carbon nanotubes, Functionalization, Cysteamine, Surface modification, Nanocomposite, Thiol, CNT
1. Introduction
Nanotechnology is significantly impressive Science and Economy in the 21st century [1]. Carbon, in different forms, has been long used as the main constituent material of solid electrodes as a further too metal electrodes [2]. After the first Iijima elucidation of their structures in 1991 [3], carbon nanotubes have attracted considerable interdisciplinary interest [4]. Carbon nanotubes are promising additives for thermoplastics, due to their superior mechanical, thermal, magnetic and electrical properties [5]. To optimize the potential applications of carbon nanotubes, it is essential to modify the carbon nanotubes with functional groups and/or nanoparticles in order to integrate the carbon nanotubes into desired structures or attach suitable nanostructures to them [6]. Carbon nanotubes possess high flexibility, large aspect ratios (Normally >1000), unique internal structures, electrical conductivity, high chemical activity, low mass density, high electro active surface area, thermal stability and great mechanical strength [7]. CNTs have extraordinary electrical conductivity and heat conductivity and mechanical properties, they are probably the top electron field-emitter possible, and their material properties can accordingly approach closely the very high levels intrinsic to them [8]. Hence, CNT’s have received considerable attention for usage in chemistry and environmental remediation [9]. CNT’s represent an exquisite class of nanomaterials that stepped into the nanomedicine arena not more than a decade behind [10]. The two main types of carbon nanotubes are the single-walled carbon nanotubes (SWCNT) and multi-walled carbon nanotubes (MWCNT), yet there are some other rare types such as fullerite, torus, and nanoknot [11].

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Surface functional groups can modify the surface charge, functionality and reactivity of the surface, and increase the stability, and dispensability of Different materials [12-13]. Organic sulfur compounds are wide-spreading in numerous natural products and widely used as multiple artificial chemicals [14]. The structure and surface chemistry of organic thin films is a research region related to several interfacial processes, including biological events, lubrication, adhesion, wettability, corrosion, electrochemistry, and microelectronic fabrication. To acquire the optimum performance of a material or device in one of these applications, the organic thin film must be prepared with the right type, concentration, and arrangement of functional handle. Functionalization of carbon nanotubes is found to be an efficient way of modification processes which in public is divided in two main categories: noncovalent and covalent. Covalent functionalization is an irretrievable process of appendage on the nanotube walls or tips it is based on the formation of a covalent coupling between functional entities and the carbon skeleton of nanotubes. Non-covalent functionalization is based on supramolecular complexation using different adsorption forces, such as van der Waals, hydrogen bonds, electrostatic force and π-π stacking interactions. [57.15-55-56].
Thiols are the maximum reactive nucleophilic reagents among altogether the biological models investigated [16]. Thiol group is an alright ligand because of its strong affinity to various heavy metal ions as a result of Lewis acid–base interactions [17]. To various heavy metal ions as a result of Lewis acid–base interactions [3].
Thiol Derivatives paper

General formula [14]

1

11

2

12

3

13

4

14

5

15

6

16

7

17

8

18

9

19

10

20

Cysteamine an aminothiol, is used to decrease tissue cystine content in patients with nephropathic cystinosis, an autosomal recessive lysosomal storage disorder in which intracellular cystine accumulates due to impaired redeploy out of lysosomes [18]. Cysteamine is a sulfhydryl containing compound which appears to arise from the decarboxylation of cysteine or the breakdown of pantetheine [19].
Scheme 1. Is a schematic Cysteamine. [20]

Scheme 1. Cysteamine

Public Name

IUPAC Name

Other Names

Molecular Formula

Molar Mass ()

Melting Point (oK)

Family

Cysteamine

2-aminoethanethiol

β-mercaptoethylamine
2-aminoethanethiol
2-mercaptoethylamine
Decarboxycysteine
Thioethanolamine
Mercaptamine

77.15

368 to 370

Amino Acid

Table 2: Structure and characteristics of Cysteamine [21]
Cysteamine () is one of the simplest molecules able to bond with the each atoms surface through its sulfur and nitrogen atoms and a prerequisite for the design of compact monolayers with acceptable properties is a fundamental understanding of the forces captive in the self-assembly process, and the characterization of the film at the molecular level [22].
Cysteamine as drug applications that have been noted in the table 3 below:

sickness

Description

Huntington’s disease (HD)

HD a neurodegenerative genetic disturbance that affects muscle coordination and leads to psychic decline and behavioral symptoms [23].

Parkinson’s disease (PD)

PD is a putrefactive disturbance of the central nervous system [24].

Non-alcoholic fatty liver disease (NAFLD)

NAFLD is one reason a fatty liver, occurring when fat is entrusted in the liver not due to excessive alcohol use [25].

Malaria

Malaria is a mosquito-borne infected illness of humans and other animals caused by parasitic protozoans (a type of single cell microorganism) of the Plasmodium type [26].

Cancer

It was appointed in 1994 that the addition of cysteamine to astrocyte culture medium resulted in increased mitochondrial autophagy [27].

Table 3
In this study, we functionalized multi-walled carbon nanotubes with carboxyl group and thiol-derivatized via condensation reaction between carboxylated-MWCNT powders and Cysteamine. Infrared (IR) spectroscopy, XRD, SEM, TEM and TGA were used to characterize the presence of Cysteamine on the MWCNT-COOH surface.
2. Experimental Procedures
2.1. Materials
Multi-walled carbon nanotubes (MWCNT’s) with Purity 95 %, outer diameter and length and manufacturing method catalytic chemical vapor deposition were purchased from US Research Nanomaterials, Inc. Sulfuric acid (97 %, AR grade) and nitric acid (37%, AR grade) were purchased from Sigma-Aldrich. N,N-dimethylformamide (DMF:98%), 1-ethyl-(3-3’-dimethylaminopropyl) carbodiimide (EDC: 97%), N-hydroxysuccinimide (NHS: 99%) were purchased from Merck Millipore and Cysteamine hydrochloride (99%) were purchased from sigma Aldrich and used as received unless otherwise stated.
2.2 Characterization methods
2.2.1 X-ray diffraction (XRD)
X-ray diffraction studies were carried out with an X-ray diffractometer (Model No. D8-Advance, Bruker AXS).
2.1.2 Fourier transform infrared spectroscopy (FTIR)
The functional groups on the MWCNT’s surface were determined using Fourier transform infrared FTIR method (VERTEX 70, Brucker). FTIR spectrum of MWCNT’S was recorded in the range of 4000– 400 using pellets method.
2.2.3 Transmission electron microscopy (TEM)
The morphologies and sizes of the nano-structures were characterized by transmission electron microscope “TEM” (PHILIPS EM 208).
2.2.4 Thermogravimetric analysis (TGA)
Thermogravimetric analysis (TGA) was carried out using a TG Labsys DSC, Setaram.
2.2.5 Scanning electron microscope (SEM)
The size and morphology of MWCNT’s was investigated by high-resolution transmission electron microscopy (VEGA3, TESCAN).
2.3 Synthesis method
At first [1] (1g) was treated with 20% hydrochloric acid for 120 min sonication, to remove impurities such as residual catalysts and amorphous carbons in the phase of synthesis , Then the sample was filtered with Millipore membrane filter 0.22 and washed many successive times with distilled water.
2.3.1 Oxidation of MWCNTs
Multi-walled carbon nanotubes was synthesized by a formerly reported method [52-53]. 0.75 g of pristine MWCNTs was added to 180ml mixture of concentrated HNO3 and H2SO4 (1:3, v/v) and then ultrasonicated for a course of 140 min. then mixture was transferred to a flask equipped with a condenser and was refluxed with drastic shocking at 75 for 6 h. After cooling to Ambient temperature the mixture was filtered with filters paper and filtrated solid was washed thoroughly by deionized water until the filtrate pH was close to neutral. The filter sample was then dried in a vacuum oven at 80 oC for 120 min. The sample was abbreviated as MWCNT-COOH.
2.3.2
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[1] Raw Carbon nanotubes( pure carbon nanotubes: p-MWCNT)