DOI: 10.5061/dryad.bnzs7h4gs
title: Carboxymethyl starch as a reducing and capping agent in the hydrothermal synthesis of selenium nanostructures for use with 3D-printed hydrogel carrier

description: The hydrothermal method is a cost-effective and eco-friendly route for
 preparing various nanomaterials. It can utilize a capping agent, such as a
 polysaccharide, to govern and define the nanoparticle morphology.
 Elemental selenium nanostructures (spheres and rods) were synthesized and
 stabilized using a tailor-made carboxymethyl starch (CMS, degree of
 substitution = 0.3) under hydrothermal conditions. CMS is particularly
 convenient because it acts simultaneously as the capping and reducing
 agent, as verified by several analytical techniques, while the reaction
 relies entirely on green solvents. Furthermore, the effect of sodium
 selenite concentration, reaction time, and temperature on the nanoparticle
 size, morphology, microstructure, and chemical composition was
 investigated to identify the ideal synthesis conditions. A pilot
 experiment demonstrated the feasibility of implementing the synthesized
 nanoparticles into vat photopolymerization 3D-printed hydrogel carriers
 based on 2-hydroxyethyl methacrylate (HEMA). When submersed into the
 water, the subsequent particle release was confirmed by dynamic light
 scattering (DLS), promising great potential for use in bio-3D printing and
 other biomedical applications.
description: # Carboxymethyl starch as a reducing and capping agent in the hydrothermal
 synthesis of selenium nanostructures for use with 3D-printed hydrogel
 carrier
 [https://doi.org/10.5061/dryad.bnzs7h4gs](https://doi.org/10.5061/dryad.bnzs7h4gs) This Zip file comprises data present in the Main article. Most files are .csv files with the Figure number used in the main article. A CIF file was taken from the COD (crystallography open Database) as a reference. Each folder has the experimental data files used to get the interpretation in the main articles, such as Fig1-NMR data, which has three .csv files, one named "final results.csv," which has two data sets outlined by black color box, one from the 1H NMR. Another is from the 13C NMR, where column G values and column Q values, which correspond to the particular chemical shifts, are used for calculating the degree of substitution of CMS, found from the Mnova software for NMR illustration.Another one is polysacc1HNMR.csv files comprising the 1H NMR data where column A is the chemical shift(ppm) of the number of hydrogens in the CMS, and column B is intensity. Moreover, in the polysacc13C.csv file, column A has the chemical shifts(ppm)of a number of carbon backbone, column B depicts the intensity of these carbons, and column C has zero values generated by the NMR instrument. These columns were used to plot the NMR Figure 1b. EDX data used for Fig 3 to interpret elemental analysis through SEM images are stated as 3h1%, 7h1%, and 14h1%. Fig 3.csv, here, the column A, C&E of 3h1%, 7h1%, and 14h1% is X-ray Energy (keV), and column B, D&F is the intensity as counts. The histogram for the width of the nanorod's calculation statistics is stated in the Fig 4 folder, with each sample labeled as 3h 1\_.csv,7h 1\_.csv, and 14h 1\_.csv, where each .csv file has the column M named length (nm)used for the nanorod width for the histogram and others columns has also labeled in the .csv file however did not use for plotting the Figure 4.In each .csv file in Folder fig 4, Column B is area of the nanorods (nm), Column C is Mean,Column D is standard deviation, Column E & F are minumum and maximum values of Mean, Column G is the perimeter of the nanorods(nm),Column H is designated to the angle by which measuremnet of width taken,Column I is circularity number, Column J is aspect ratio , Column K is Round shape , Column L defines solidity. Data used in Fig5, all four .csv files are separately located in a folder named Fig5, such as DTA\_fig5.csv, where the first column is dedicated to the derivative of weight%/Temperature for CMS and the second column is the temperature (°C) and the consequent column has derivate weight%/Temperature for 3h1%,7h1% and 14h1% this measurement done to find the temperature change, In FTIR Fig5.csv file first column is dedicated to the wavenumber(1/cm) and rest columns devoted to the transmittance(%) for sample CMS, 3h1%,7h1%, and 14h1%. In the TGA file fig5.csv, the first column is dedicated to the temperature(°C), and consecutive columns have the weight % for CMS, 3h1%, 7h1%, and 14h%. In the XRD file for Fig5, columns A and C&E depict the diffraction angle (2Theta) range used for all samples, and subsequent columns B, D&F have the intensity(cps) for all the samples CMS, 3h1%, 7h1%, and 14h 1%. The histogram used in Fig6 was generated from the Origin using the width sizes(nm)of nanorods using the STEM images; individual histogram data is available in the Fig6stastics.csv file, where first column depicted the width of the nanorode STEM images obtained from sample 7h1%cms1% Se ion in nanometers, and consequently for 7h 1%CMS 0.5% Se ion and 7h1%CMS 0.25% Se ion. In Folder Fig7, all data used for Fig 7 in the main article are placed in this folder with their name as a .csv file. In the first column of Fig 7 FTIR .csv file, the first column depicts the wavenumber(1/cm) range used for the sample 7h0.25%Se 1% CMS. The next column is shown for the transmittance(%), the second column is for the wavenumber(1/cm), column D is for the transmittance (%)for sample 7h0.5%Se 1% CMS, column E depicted for the wavenumber(1/cm) and Column F for the transmittance(%) for the sample 7h1%Se 1% CMS. Fig 7a.csv shows the DLS date, where column A depicts the hydrodynamic size of the nanorods(nm) of sample 7h0.25%Se 1% CMS, column B is the intensity distribution(%), and column C for the size of the nanorods(nm) of sample 7h0.5%Se 1% CMS and column D intensity(%) and column E and F for the sample 7h1%Se 1% CMS. In Fig7 XRD, Coulmn A depicted the 2-theta and column B for the x-ray diffraction intensity (cps) for the sample 7h0.25%Se 1% CMS followed by the other samples 7h0.5%Se 1% CMSand 7h1%Se 1% CMS. In Fig 7 Zeta potential.csv file, which shows the stability of the nanostructures, column A represents the zeta potential(mV) and Column B for the intensity distribution data(counts) for the sample 7h 0.25% Se ion 1% CMS, consequently columns C & D for the Sample 7h 0.5% Se ion 1% CMS and columns E & F dedicated for the sample 7h 1% Se ion 1% CMS. Folder Fig 9 comprises XPS data, where each .csv file has names with the figure number and each .csv file has labeled the units with the column and in Fig 9a.csv for the wide XPS spectra of all samples where column A depicted the binding energy(eV) for all the three samples and Coulmn B, C & D represented the Intensities(cps) for samples 7h 0.25% Se ion 1% CMS,7h 0.5% Se ion 1% CMS & 7h 1% Se ion 1% CMS. Fig9b.csv showed the elemental spectra of Se(3d), where column A depicted the Binding energy(eV) for the sample 7h 0.25% Se ion 1% CMS, and column B is the respective intensity(cps), columns C & D dedicated to the sample 7h 0.5% Se ion 1% CMS and columns E& F for the sample 7h 1% Se ion 1% CMS respectively. In Fig9c, XPS spectra of Carbon(1s), where columns A, C & E are dedicated to the binding energy(eV) for samples 7h 0.25% Se ion 1% CMS,7h 0.5% Se ion 1% CMS & 7h 1% Se ion 1% CMS and columns B, D & F intensity(cps) of all three samples respectively. EDX data used for Fig10 is stored in a .csv file named Fig10.csv, where columns A, C &E are X-ray energy (keV) for the samples 3h 100°C,3h135°C and 3h 160°C.Columns B, D & F are the intensity counts for the respective samples 3h 100°C,3h 135°C & 3h 160°C. DLS data used in Fig11 are placed in a .xlsx file named fig11DLS SLNS.xlsx.xlsx, where column A depicts the hydrodynamic size distribution in (nm) of selenium nanoparticles, and column B represents the intensity in (%).