Progress 10/01/07 to 09/30/12
Outputs
OUTPUTS: This year, we continued our work on optimization of TiCl4 plasma-treated to improve self-cleaning and flame resistance of Cellulosic based materials. After plasma treatment, samples were processed and run on the 45 degree angle burn test. The samples were prepared with 40 mTorr of TiCl4 up to 204 mTorr with a base pressure of 27 mTorr and additional Argon gas making up the difference. After reacting for 10 minutes at 100kW operating power for the plasma, the plasma was stopped, and the chamber gas was replaced by O2 gas for varying lengths of time. Some samples were prepared with 5 minutes of O2 following the reaction, the second group of samples was prepared with 7 minutes of O2 following the reaction, and the third group of samples were prepared with 10 minutes of O2 following the reaction. The treatments on the cotton with TiCl4 were run with a base pressure of 27 mTorr, 154 mTorr of O2, and 23 mTorr of TiCl4. The second group was run with a base pressure of 27 mTorr, 164 mTorr of O2, and 17 mTorr of TiCl4. Two groups were run under those conditions. FTIR and Raman scans of the samples were taken. Sodium Silicate Samples were run on SEM-EDS. The concentrations were as follows: 1.3%, 2.6%, and 5.2% with a control sample of untreated cotton. Two samples from each concentration were taken, one before plasma treatment and the other after. All samples were washed 3 times in DI water for 30 minutes by ultrasound bath prior to being mounted; sputter coated, and run on the SEM. The EDS data shows an image of the EDS scan with the overlay of the response from the silicon emission. The overlay seems to show a higher count of Si on those treated with plasma versus those untreated. It seems there is some residual noise response for Si on the control sample. The results were disseminated in the Hatch multistate annual meeting. PARTICIPANTS: The participants were: Majid Sarmadi as PI; Philip Gonzales, PH.D Student; Sorin Manolache, PhD, assistant scientist; Plasma Center UW-Madison. Mr. Glen Finkel from a US based company "Pureti Inc." is interested in some of our results and after lengthy scientific discussion, the company is evaluating ways of collaboration on this area. TARGET AUDIENCES: Scientific community, industry, and graduate and undergraduate students. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
Student training was one of the most important outcomes of this project. Also, the results were shared between the researchers of different universities who were a part of the project. The resources provided by this project were essential for graduate student training and performing the research. We have found some improvement in self cleaning and flame resistance.
Publications
- No publications reported this period
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Progress 01/01/11 to 12/31/11
Outputs
OUTPUTS: The main objective of the period was training a skilled student to perform sound research. Therefore the following training were given: For work with the parallel plate plasma processor, training was given for the use of Argon plasma under vacuum as well as the construction of the processor and the parameters for the use of plasma in the incorporation of the inorganic to the surface. Training was also given for the use and operation of the Soxhlet extraction of organic compounds from solid material for purifying the polymeric cloth. Characterization of the interaction of the material with the surface of the cloth was performed. FTIR spectroscopy and Raman spectroscopy instrument training were performed. Analysis of various samples through FTIR spectroscopy showd the presence of silicate on the surface of the cloth, however, there is not a clear difference in the FTIR scans between the samples that have and have not been treated with plasma. Raman spectroscopy showed no clear correlation between the samples, however, due to the nature of Raman scattering, this analysis could prove fruitful in further studies utilizing different inorganic flame retardants. Training with the 45 degree angle Auto-Flame chamber was performed as the burning behavior was tested for each of the samples. Data from the samples run for burning behavior analysis correlated with the data from previous studies, showing that the plasma treated samples had a longer flame spread time than the samples untreated with plasma. Further surface analysis of the samples will take place via SEM-EDS. Virtual training has been performed for organic samples under general operating parameters used in an SEM. These tests should characterize the nature of the surface with an SEM image as well as obtain an elemental map of a selected area, showing the presence of the inorganic compound at different points on the substrate. PARTICIPANTS: The role of the PI was to set the general research direction and oversee the progress, train student, and review the weekly research report and to help the PhD. The student solves daily research problems when needed. The Role of the PhD. Student was to perform the research and discuss the outcome with the PI. The equipment trainings were given at UW-Plasma Center and the UW-Materials Center. TARGET AUDIENCES: Not relevant to this project. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
Improved skills of the student and increased knowledge of decision-making in area of plasma processing, FTIR analysis, Soxhlet extraction,45 degree angle Auto-Flame chamber and Raman spectroscopy instrument were the main outcomes.
Publications
- Totolin,V., Sarmadi, M., Manolache, S., and Denes,F. S.,(2011) Environmentally Friendly Flame Retardant Materials Produced by Atmospheric Pressure Plasma Modifications, Journal of Applied Polymer Science, Vol. 124, Issue 1, pp. 116-122.
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Progress 01/01/10 to 12/31/10
Outputs
OUTPUTS: The outcomes of this research have been disseminated by presenting and sharing with the Multistate Hatch researchers, other scientists at national scientific conferences, and by publishing in the scientific journal, and presenting them in a dissertation. A trained PhD student is one of the important outcomes. PARTICIPANTS: Dr. Vladimir Totolin was trained, wrote his dissertation on this subject and received his PhD from UW-Madison in 2010. Other Collaborators were Dr. Sorin Manolache from Center for Plasma-Aided Manufacturing and Professor Denes from Department of Biological System Engineering. TARGET AUDIENCES: The target audience for the outcome of this research include: textile industry, researchers in this field and faculty of universities who teach this subject PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
The objective of this work was to investigate plasma modification of viscose for environmentally friendly flame retardant cellulosic materials. Sodium silicate layers were pre-deposited onto viscose and cotton flannel substrates and grafted / cross-linked using atmospheric pressure plasma. The modified cellulosic fabrics tested with the automated 45o angle test chamber showed significant improvement in their flame retardant properties. Analysis conducted by TGA and DSC exhibited enhanced thermal stability of the treated fabrics. Furthermore, the surface analysis (XPS and SEM) confirmed the presence of the SiO2 network attached to the substrate even after intense ultrasound washes. These results could not be achieved without the Hatch support. Keywords: flame retardant, viscose, cotton flannel, atmospheric pressure plasma, coatings
Publications
- V. Totolin, M. Sarmadi, S. Manolache, and F. S. Denes 2010,Atmospheric Pressure Plasma Enhanced Synthesis of Flame Retardant Cellulosic Materials, Journal of Applied Polymer Science,Vol.117, 1,
- V. Totolin, 2010, PhD. dissertation. Plasma-enhanced Synthesis of Green Flame Retardant Cellulosic Materials, UW-Madison.
- V. Totolin, M. Sarmadi, S. Manolache, and F. S. Denes, May 2010, Obtaining Flame Retardant Cotton Fabric from Silicone Based Compounds by Plasma Processes, AATCC International Conference, Atlanta. (Modified the published paper for the conference proceedings ).
- Totolin, M. Sarmadi, S. Manolache, and F. S. Denes, March 2010, Atmospheric Pressure Plasma Enhanced Synthesis of Green Flame Retardant Cellulosic Materials, ACS National Meeting & exposition, San Francisco, (Abstract)
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Progress 01/01/09 to 12/31/09
Outputs
OUTPUTS: Flame retardant cellulosic materials have been produced using a silicon dioxide (SiO2) network coating. SiO2 network armor was prepared through hydrolysis and condensation of the precursor tetraethyl orthosilicate (TEOS), prior coating the substrates, and was cross linked on the surface of the substrates using atmospheric pressure plasma (APP) technique. The cellulosic substrate employed was bleached desized cotton print cloth (78 x 76), weight = 102 g/m2 purchased from Test Fabrics and cut in 2x6" samples. Prior the treatment, the cotton samples were Soxhlet extracted in a toluene/ ethanol mixture (1:2 ratio) for 24 hours to remove the extractives present in cellulose. Due to protection effects of the SiO2 network armor, the cellulosic based fibers exhibit enhanced thermal properties (characterized by TGA and DSC) and improved flame retardancy (proven by ASTM D1230- 99). Furthermore, the surface analysis (XPS and SEM) confirmed the presence of the SiO2 network attached to the substrates even after intense ultrasound washes. PARTICIPANTS: Vladimir Totolin, Ph.D. student; Sarmadi, Majid, Faculty PI; Manolache S.O., collaborator from UW-Plasma Center; Denes, F., collaborator from UW-Plasma Center TARGET AUDIENCES: This information provides basic and applied knowledge in the area of flame retardant textile materials.The target audiences include: Faculty, students and industries in the textile and related fields. PROJECT MODIFICATIONS: Not relevant to this project.
Impacts
A refereed journal article is one of the outcomes of this project. In this publication, a new method for making textile materials flame retardant is described which adds to the basic and applied knowledge in this area. The treated fabrics have SiO2 network armor, and exhibit enhanced thermal properties.
Publications
- Vladimir Totolin, M. Sarmadi, S.O. Manolache and F.S. Denes, 2009, Low Pressure, Non-Equilibrium Plasma assisted Generation of Flame Retardant Cotton, AATCC- Review, Vol. 9, 6.
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Progress 01/01/08 to 12/31/08
Outputs
OUTPUTS: One of the objectives of this project was to generate antimicrobial treatments. This objective has been archived. This information was disseminated in 2008 by presenting papers at International conferences and publishing the outcomes in the referred journals. Another objective is to generate durable flame retardant treatment on cotton fabrics. The work on this objective is in the progress. The preliminary results have been presented at a international conference and a manuscript is submitted to disseminate the information. PARTICIPANTS: In addition to myself, my Ph.D. student Valdimir Totolin and S. Manolache and F.Denes from Plasma Center. Other participants are the members of the Multistate research committee. TARGET AUDIENCES: The target audiences for this project are the textile industry, educational institutes and homeland security. PROJECT MODIFICATIONS: Nothing significant to report during this reporting period.
Impacts
One of the objective of this project is to generate durable flame retardant treatment on cotton fabrics. Sodium silicate layers were pre-deposited onto clean cotton substrates and crosslinked using low pressure, non-equilibrium oxygen plasma. Prior the deposition the cotton samples were Soxhlet extracted in acetone for 6 hours to insure a clean surface. A statistical design of experiments was used to optimize the plasma parameters. Cotton samples were tested for flammability with an automatic 45o angle flammability test chamber. TGA analyses indicate low quantity of coating material. Aging tests were also conducted to test the coating resistance to the accelerated laundry technique. The surface of the untreated and treated samples was characterized by XPS, ATR/ FTIR and SEM.
Publications
- S. N. Jampala, S. Manolache, M. Sarmadi, F. Denes. 2008. Surface Functionalization by RF Plasma Deposition of Ethylene Diamine, Acrylonitrile and Acetonitrile. Journal of Applied Polymer Science Vol. 107, No. 3, pp. 1686-1695.
- S. N. Jampala, M. Sarmadi, E.B. Somers, A. Wong, F. S. Denes. 2008. Plasma-Enhanced Synthesis of Quaternary Ammonium Thin Layers on Stainless Steel and Cellulose Surfaces, Lanmuir, Vol. 24, pp 8583-8591.
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Progress 01/01/07 to 12/31/07
Outputs
OUTPUTS: The first par of this work focused on the development of surface layers that kill bacteria on contact using cold plasma techniques. The successful grafting of Quaternary ammonium (QA) groups on stainless still (SS) and cellulose-based surfaces rendered them bactericidal against Gram-positive S. aureus and Gram-negative K. pneumoniae. The second part of this research focused on making cotton fabrics flame retardant. Preliminary work is promising, but much work is needed before we be able to report.
PARTICIPANTS: Soujanya N. Jampala, Ph.D. Student; Professor Sarmadi,M., UW-Madison; S. Manolache, Researcher, Plasma Center; Professor A. Wong, UW-Madison; Professor Denes, UW-Madison; F, K. Leonas, University of Georgia-Athens; Vladimir Totolin, Ph.D student, UW-Madison.
TARGET AUDIENCES: Target Audiences are: Textile Industry; Textile Finishing Industry; Cotton Growing Farmers (value added products); Plasma Industry
Impacts
Thin macromolecular films were deposited in ED, AN, and AcN plasma to functionalize surfaces with reactive amine groups. The effect of RF plasma power and frequency (40 kHz and 13.56 MHz) on surface chemistry was investigated. Significant changes in surface chemistry of ED, and AN plasma deposited films with increase in RF plasma power and frequency (40 kHz and 13.56 MHz) were observed. AcN plasma molecular fragmentation was found to be independent of plasma conditions. The films deposited in continuous mode at 13.56 MHz resulted in higher concentrations of amine groups and ED plasma deposited film was used for grafting of QA groups. A pretreatment involving O2- and HMDSO plasma treatments facilitated the adhesion of ED plasma film on SS surfaces. QA groups were successfully synthesized by reacting ED plasma films with an alkyl bromide. An additional step of methylation increased the concentration of QA groups and enhanced the bactericidal properties of the surfaces.
Bactericidal efficacies as high as 99.9% for S. aureus and 98% for K. pneumoniae were exhibited in modified SS and cotton fabric surfaces. The biocidal activity of QA groups was dependent on the alkyl chain length in the structures. The alkyl bromides with one to eighteen carbons were used in the quaternization reaction. The maximal activity against S. aureus was found with hexyl chains and the one with dodecyl chains were most potent against K. pneumoniae.
Publications
- Soujanya Jampala. 2007.Plasma Treatment for Textile Surfaces that Kill Microorganism on Contact. Ph.D. Dissertation, UW-Madison.
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