User Manual: - Electrospinz
Contents
1. Electric Field 0 2 Doshi and Reneker 1995 3 2 kV cm Yarin and Zussman 2004 Page 27 of 43 References Bhattarai et al 2005 Deitzel et al 2001a Deitzel et al 2001b Doshi and Reneker 1995 Fong et al 1999 Hohman et al 2001 Huang et al 2003 Kessick et al 2004 Kessick and Tepper 2004 Kidoaki et al 2005 Megelski et al 2002 Reneker et al 2000 Shin et al 2001a Shin et al 2001b Son et al 2004a Spivak et al 2000 Sun et al 2006 Theron et al 2005 Wang et al 2004 Yarin et al 2001 Yarin and Zussman 2004 Solvents Water Koski et al 2004 Ethanol Water 1 1 Theron et al 2004 Aqueous Acetic Acid Duan et al 2006 Polyvinyl alcohol PVOH Typical Processing Parameters Concentration 8 Wang et al 2006b Molecular Weight 80 000 Guan et al 2003b Voltage 20kV Ding et al 2002 Distance 10cm Son et al 2005 Electric Field 1 5 kV cm Duan et al 2006 Processing Parameters Range Conc 4 1 Shao et al 2003 18 Ding et al 2002 Conc 2 8e7 mol L Ding et al 2002 2 9e mol L Lee et al 2004 Mw 10 000 Theron et al 2004 185 000 Koski et al 2004 Voltage 5kV Zhang et d 2005 100kV Theron et al 2004 Distance 3 5 cm Morozov et al 1998 25 cm Wang et al 2004 Electric Field 0 3 kV cm Zhang et al 2005 4 kV cm Lee et al 2004 Page2. Toluene Methanol 1 1 Dichloromethane M ethanol 3 1 Acetone Theron et al 2004 Biopolymers Polycaprolactone PCL Typical Processing Parameters Concentration 10 Theron et al 2004 Molecular Weight 80 000 Zhang et al 2004 Voltage 15 kV Dalton et al 2005 Distance 12 cm Zhang et al 2004 Electric Field 1 kV cm Duling et al 2008 Processing Parameters Range Conc 5 Lee et al 2008 12 Fridrikh et al 2003 Conc 2 5e Lee et al 2008 1 3e Zhang et al 2004 My 80 000 Theron et al 2004 200 000 Lee et al 2008 Voltage 12 kV Theron et al 2004 20 kV Lee et al 2008 Distance 10 cm Lee et d 2008 15cm Dalton et al 2005 Electric Field 1 kV cm Dalton et al 2005 2 kV cm Lee et al 2008 Page 31 of 43 References Dalton et al 2005 Fridrikh et al 2003 Theron et al 2004 Zhang et al 2004 Lee et al 2008 Duling et al 2008 Solvents N N Dimethylformamide DMF N N Dimethylformamide DMF Methylene chloride Zong et al 2002 Dichloromethane Shenoy et al 2005a Dichloroethane Chloroform Zeng et al 2003a Polylactic acid PLA PLLA PDLA Typical Processing Parameters Concentration 10 Zeng et al 2003a Molecular 109 000 Zong et al 2002 Weight Voltage 25 kV Ko et al 2003 Distance 15 cm Zong et al
3. Biodegradable electrospun fibers for drug delivery Journal of Controlled Release 92 227 231 ZHANG C YUAN X WU L HAN Y amp SHENG J 2005 Study on morphology of electrospun poly vinyl alcohol mats European Polymer Journal 41 423 432 ZHANG Y HUANG Z M XU X LIM C T amp RAMAKRISHNA S 2004 Preparation of Core Shell Structured PCL r Gelatin Bi Component Nanofibers by Coaxial Electrospinning Chemistry of Materials 16 3406 3409 ZONG X KIM K FANG D RAN S HSIAO B S amp CHU B 2002 Structure and process relationship of electrospun bioabsorbable nanofiber membranes Polymer 43 4403 4412 Page 43 of 43
4. 2002 Electric Field 2 kV cm Zong et al 2002 Processing Parameters Range Conc 3 Shenoy et al 2005a 40 Zong et al 2002 Conc 4 5e Shenoy et al 2005a 4 0e Zong et al 2002 Mw 48 000 Zeng et al 2003a 670 000 Shenoy et al 2005a Voltage 20 kV Zong et al 2002 41 kV Zeng et al 2003b Distance 15 cm Ko et al 2003 20 cm Zeng et al 2003b Electric Field 0 75 kV cm Zeng et al 2003a 2 kV cm Zeng et al 2003b Page 32 of 43 References Ko et al 2003 Zong et al 2002 Zeng et al 2003b Shenoy et al 2005a 2003a Zeng et al Solvents Acetone Dimethylac etimide DMAc 2 1 Ding et al 2004 Acetone water 5 20 wt water Son et al 2004b Acetic Acid Han et al 2008 Dimethylformamide Tungprapa et al 2007 Cellulose Acetate CAc Typical Processing Parameters Concentration 16 Tungprapa et al 2007 Molecular 30 000 Han et al 2008 Weight Voltage 16 kV Chen et al 2008 Distance 15 cm Ding et al 2004 Electric Field 1 3 kV cm Ding et al 2004 Processing Parameters Range Conc 396 Chen et al 2008 2196 Son et al 2004b Conc 6 0e Chen et al 2008 7 0e Son et al 2004b My 30 000 Son et al 2004b 50 000 Chen et al 2008 Voltage 8 kV Son et al 2004b 25 kV Han et al 2008 Distance 6 cm Son
5. 28 of 43 References Ding et al 2002 Ding et al 2004 Duan et al 2006 Guan et al 2003a Guan et al 2003b Guan et al 2003c Koski et al 2004 Lee et al 2004 Morozov et al 1998 Ohkawa et al 2004 Ristolainen et al 2006 Shao et al 2003 Shenoy et al 2005b Son et al 2005 Theron et al 2004 Wang et al 2006b Wang et al 2004 Yao et al 2003 Zhang et al 2005 Solvents N N Dimethylformamide Toluene Megelski et 2002 al Carbon Disulfide CS2 Eda et al 2007b Chloroform Tetrahydrofuran THF Methylethylketone Jarusuwannapoom et al 2005 Acetic Acid Wannatong et al 2004 Polystyrene PS Typical Processing Parameters Concentration 20 Shin et al 2005 Molecular Weight 200 000 300 000 Jarusuwannapoom et al 2005 Voltage 30 kV Eda et al 2007b Distance 15 cm Wang et al 2006a Electric Field 1 kV cm Sundaray et al 2004 Processing Parameters Range Conc 2 5 Eda et al 2007a 35 Casper et al 2004 Conc 1 4e mol L Eda et al 2007a 1 7e gt mol L Casper et al 2004 Mw 4 000 Wang et al 2006a 1 880 000 Wang et al 2006a Voltage 3 kV Sundaray et al 2004 30 kV Wannatong et al 2004 Distance 3 cm Sundaray et al 2004 35 cm Casper et al 2004 Electric Field 0 14 kV cm Megelski et al 2002 3 kV cm Eda et al 2
6. 40 1261 1268 DING B KIMURA E SATO T FUJITA S amp SHIRATORI S 2004 Fabrication of blend biodegradable nanofibrous nonwoven mats via multi jet electrospinning Polymer 45 1895 1902 DOSHI J amp RENEKER D H 1995 Electrospinning Process and Applications of Electrospun Fibers Journal of Electrostatics 35 151 160 DUAN B YUAN X ZHU Y ZHANG Y LI X ZHANG Y amp YAO K 2006 A nanofibrous composite membrane of PLGA chitosan PVA prepared by electrospinning European Polymer Journal 42 2013 2022 Page 37 of 43 DULING R R DUPAIX R B KATSUBE N amp LANNUTTI J 2008 Mechanical characterization of electrospun polycaprolactone PCL A potential scaffold for tissue engineering Journal of Biomechanical Engineering Transactions of the Asme 130 EDA G LIU J amp SHIVKUMAR S 2007a Flight path of electrospun polystyrene solutions Effects of molecular weight and concentration Materials Letters 61 1451 1455 EDA G LIU J amp SHIVKUMAR S 2007b Solvent effects on jet evolution during electrospinning of semi dilute polystyrene solutions European polymer journal 43 1154 1167 FONG H CHUN I amp RENEKER D H 1999 Beaded nanofibers formed during electrospinning Polymer 40 4585 4592 FONG H amp RENEKER D H 1999 Elastomeric nanofibers of styrene butadiene styrene triblock copolymer Journal of Polymer Science Part B Polymer Physics 37 3488 3
7. LU X ZHAO Y amp WANG C 2006b Preparation and characterization of ZnS Cu PVA composite nanofibers via electrospinning Materials Letters 60 2480 2484 Page 42 of 43 WANG M SINGH H HATTON T A amp RUTLEDGE G C 2004 Field responsive superparamagnetic composite nanofibers by electrospinning Polymer 45 5505 5514 WANNATONG L SIRIVAT A amp SUPAPHOL P 2004 Effects of solvents on electrospun polymeric fibers preliminary study on polystyrene Polymer International 53 1851 1859 YAO C LI X S amp SONG T Y 2007 Electrospinning and crossfinking of Zein nanofiber mats Journal of Applied Polymer Science 103 380 385 YAO L HAAS T W GUISEPPI ELIE A BOWLIN G L SIMPSON D G amp WNEK G E 2003 Electrospinning and stabilization of fully hydrolyzed poly vinyl alcohol fibers Chemistry of Materials 15 1860 1864 YARIN A L KOOMBHONGSE S amp RENEKER D H 2001 Taylor cone and jetting from liquid droplets in electrospinning of nanofibers Journal of Applied Physics 90 4836 4845 YARIN A L amp ZUSSMAN E 2004 Upward needleless electrospinning of multiple nanofibers Polymer 45 2977 2980 ZENG J CHEN X XU X LIANG Q BIAN X YANG L amp JING X 2003a Ultrafine Fibers Electrospun from Biodegradable Polymers Journal of Applied Polymer Science 89 1085 1092 ZENG J XU X CHEN X LIANG Q BIAN X YANG L amp JING X 2003b
8. et al 2004b 45 cm Chen et al 2008 Electric Field 0 4 kV cm Chen et al 2008 2 5 kV cm Han et al 2008 Page 33 of 43 References Ding et al 2004 Son et al 2004b Chen et al 2008 Han et al 2008 Tungprapa et al 2007 Solvents 1 1 1 3 3 3 Hexafluoro 2 propanol Li et al 2006 2 2 2 trifluoroethanol Huang et al 2004 Acetic Acid Formic Acid Songchotikunpan et al 2008 Gelatine Typical Processing Parameters Concentration 10 Zhang et al 2004 Voltage 15 kV Zhang et al 2004 Distance 12 cm Huang et al 2004 Electric Field 1 kV cm Li et al 2006 Processing Parameters Range Conc 5 Huang et al 2004 2996 Songchotikunpan et al 2008 Voltage 10 kV Li et al 2006 28 kV Powell and Boyce 2008 Distance 10 cm Li et d 2006 15 cm Songchotikunpan et al 2008 Electric Field 0 8 kV cm Huang et al 2004 1 3 kV cm Huang et al 2004 Page 34 of 43 References Huang et al 2004 Li et al 2006 Zhang et al 2004 Songchotikunpan et al 2008 Powell and Boyce 2008 Solvents Ethanol Water 4 1 Miyoshi et al 2005 Acetic Acid Isopropyl Alcohol Water 4 1 Ethanol Water 3 2 Selling et al 2007 Dimethylformamide Jiang et al 2007 Typical Processing Parameters Concentration 25 Miyoshi et al 2005 Voltage 20 kV Jiang et al
9. of this manual is to explain safe operating procedures for the electrospinning machine ES4 and ES1a 1 2 Principle Electrospinning uses an electrical charge to draw very fine micro or nanofibres from a polymer in a liquid solution or melt The process is non invasive and does not require the use of coagulation chemistry or high temperatures to produce solid threads from solution This makes the process particularly suited to the production of fibres using large and complex molecules When a sufficiently high voltage is applied to a liquid droplet the body of the liquid becomes charged and electrostatic repulsion counteracts the surface tension and droplet is stretched and a Taylor cone appears at a critical point a stream of liquid erupts from the surface at the tip of the Taylor cone If the molecular cohesion of the liquid is sufficiently high stream breakup does not occur if it does droplets are electrosprayed and a charged liquid jet is formed As the jet dries out in flight the mode of current flow changes from ohmic to convective as the charge migrates to the surface of the fibre The jet is then elongated by a whipping process caused by electrostatic repulsion initiated at small bends in the fibre until it is finally deposited on the grounded collector The elongation and thinning of the fibre resulting from this bending instability leads to the formation of uniform fibres with nanometre scale diameters A typical electros
10. supply to contend with in terms of risk of ventricular fibrillation disruption of the activity of the heart Cf Appendix II Why doesn t the machine need an enclosure to be safe Page 18 of 43 Glossary Aligned fibres electrospun nanofibres which are parallel to each other Applied Voltage Potential Difference The voltage applied to the solution via the control box A typical voltage used for electrospinning is 10kV Control Box regulates the applied voltage and therefore the electrospinning process Deposition Process how the fibres are depositing on the target Earth Stud Electric Current Collector connected to the earth this device allows the current to circulate and therefore electrospinning to occur This system is also designed to electrically discharge each metallic part of the platform is an important safety part of the machine Electrospinning The operation of creating nanofibres from a polymer dissolved in a solution by applying a voltage to that liquid Electrospinning Jet the jet formed by the liquid at the tip of the needle between the Taylor cone and the whipping instability Laboratory Electrospinning Platform the name of the machine for electrospinning platform indicates that the machine is designed to be modified for research purposes Electrospun nanofibres nanofibres which are created through an electrospinning process Nanofibres are considered to be less than 100nm in diameter Elect
11. the naked eye Normally only a very slight increase in voltage will initiate the spinning process The Taylor Cone a typical stable jet If spinning is continued too long then the build up of fibre on the target can be enough to insulate the target and fibres may be deposited in other areas Page 13 of 43 3 5 Maintenance Cleaning A Remove the header tank hose and spinning tip Move these to the cleaning area B Remove the spinning bush use the 10mm spanner if required C Do not remove the brass spinning bush holder D The spinning bush is made from stainless steel and should be thoroughly washed and dried before reassembly E The spinning tip may be cleaned but is designed as a disposable item F Clean the base of the machine with a damp cloth or a cloth dampened with a little solvent Be careful with solvents around the plastic components as these may be damaged by some solvents G Reassemble in the reverse order be careful not to over tighten the nut on the spinning bush finger tight is usually enough Servicing The ES1a and ES4 have been designed to be serviced without returning it to Electrospinz Limited The electrical system must be serviced only by qualified personal and must be maintained in compliance with the relevant local legislation Replacement components are available worldwide and should be obtained locally The mechanical components should be serviced by a competent person any required s
12. 007b Page 29 of 43 References Casper et al 2004 Eda et al 2007b Eda et al 2007a Reneker and 1999 Jarusuwannapoom et al 2005 Megelski et al 2002 Shenoy et al 2005a Shin et al 2005 2004 Wang et al 20060 Wannatong et al 2004 Fong Sundaray et al Solvents N N Dimethylformamide DMF Smit et al 2005 Polyacrylonitrile PAN Typical Processing Parameters Concentration 1096 Kim and Yang 2003 Molecular Weight 775 000 Qin et al 2004 Voltage 10 25 kV Kim and Yang 2003 Distance 16cm Samatham and Kim 2006 Electric Field 1 7 kV cm Ko et al 2003 Processing Parameters Range Conc 4 Qin et al 2007 14 Qin et al 2005 Conc 3 8e mol L Sutasinpromprae et al 2006 3 263 mol L Sutasinpromprae et al 2006 My 55 000 Sutasinpromprae et al 2006 210 000 Smit et al 2005 Voltage 5 kV Qin et al 2004 40 kV Qin et al 2007 Distance 10 cm Sutasinpromprae et al 2006 30 cm Sutasinpromprae et al 2006 Electric Field 0 3 kV cm Samatham and Kim 2006 3 kV cm Sutasinpromprae et al 2006 Page 30 of 43 References Ko et al 2003 Smit et al 2005 Sutasinpromprae et al 2006 Qin et al 2007 Kim and Yang 2003 Samatham and Kim 2006 Qin et al 2004 Qin et al 2005 Solvents Chloroform Methan ol 3 1 Dalton et al 2005
13. 2007 Distance 10 cm Selling et al 2008 Electric Field 2 kV cm Yao et al 2007 Zein Processing Parameters Range Conc 17 Selling et al 2008 50 Yao et al 2007 Voltage 8 kV Miyoshi et al 2005 40 kV Selling et al 2007 Distance 5 cm Selling et al 2007 25 cm Jiang et al 2007 Electric Field 0 5 kV cm Jiang et al 2007 4 kV cm Selling et al 2007 Page 35 of 43 References Miyoshi et al 2005 Selling et al 2007 Jiang et al 2007 Yao et al 2007 Selling et al 2008 Solvents Melt Spinning Polypropylene PP Typical Processing Parameters Polymer 285 C Lee and Obendorf 2006 Temp Molecular 200 000 Dalton et al 2007 Weight Voltage 20 kV Dalton et al 2007 Distance 4 cm Dalton et al 2007 Electric Field 5 kV cm Dalton et al 2007 Processing Parameters Range Polymer Temp 200 C Lyons et al 2004 320 C Dalton et al 2007 My 14 000 Lyons et al 2004 580 000 Lyons et al 2004 Voltage 10 kV Lee and Obendorf 2006 30 kV Lyons et al 2004 Distance 2 cm Lyons et al 2004 7 cm Lee and Obendorf 2006 Electric Field 1 4 kV cm Lee and Obendorf 2006 15 kV cm Lyons et al 2004 Page 36 of 43 References Lee and Obendorf 2006 Lyons et al 2004 Dalton et al 2007 References BHATTARAI N EDMONDSON D VEIS
14. 493 FRIDRIKH S V YU J H BRENNER M P amp RUTLEDGE G C 2003 Controlling the fiber diameter during electrospinning Physical Review Letters 90 144502 1 GUAN H SHAO C GONG B C J amp YANG X 2003a A novel method for making CuO superfine fibres via an electrospinning technique Inorganic Chemistry Communications 6 1409 1411 GUAN H SHAO C GONG B C J amp YANG X 2003b Preparation and characterization of NiO nanofibres via an electrospinning technique Inorganic Chemistry Communications 6 1302 1303 GUAN H SHAO C WEN S GONG B C J amp YANG X 2003c A novel method for preparing Co304 nanofibers by using electrospun PVA cobalt acetate composite fibers as precursor Materials Chemistry and Physics 82 1002 1006 HAN S O YOUK J H MIN K D KANG Y O amp PARK W H 2008 Electrospinning of cellulose acetate nanofibers using a mixed solvent of acetic acid water Effects of solvent composition on the fiber diameter Materials Letters 62 759 762 HOHMAN M M SHIN M RUTLEDGE G amp BRENNER M P 2001 Electrospinning and electrically forced jets Il Applications Physics of Fluids 13 2221 2236 HUANG Z M ZHANG Y Z KOTAKI M amp RAMAKRISHNA S 2003 A review on polymer nanofibers by electrospinning and their applications in nanocomposites Composites Science and Technology 63 2223 2253 Page 38 of 43 HUANG Z M ZHANG Y Z RAMAKRISH
15. EH O MATSEN F A amp ZHANG M 2005 Electrospun chitosan based nanofibers and their cellular compatibility Biomaterials 26 6176 6184 CASPER C L STEPHENS J S TASSI N G CHASE D B amp RABOLT J F 2004 Controlling Surface Morphology of Electrospun Polystyrene Fibers Effect of Humidity and Molecular Weight in the Electrospinning Process Macromolecules 37 573 578 CHEN L BROMBERG L HATTON T A amp RUTLEDGE G C 2008 Electrospun cellulose acetate fibers containing chlorhexidine as a bactericide Polymer 49 1266 1275 DALTON P D GRAFAHREND D KLINKHAMMER K KLEE D amp MOLLER M 2007 Electrospinning of polymer melts Phenomenological observations Polymer 48 6823 6833 DALTON P D KLEE D amp MOLLER M 2005 Electrospinning with dual collection rings Polymer 46 611 614 DEITZEL J M KLEINMEYER J HARRIS D amp TAN N C B 2001a Effect of processing variables on the morphology of electrospun nanofibers and textiles Polymer 42 261 272 DEITZEL J M KLEINMEYER J D HIRVONEN J K amp BECK TAN N C 2001b Controlled deposition of electrospun poly ethylene oxide fibers Polymer 42 8163 8170 DING B KIM H Y LEE S C SHAO C L LEE D R PARK S J KWAG G B amp CHOI K J 2002 Preparation and Characterization of a Nanoscale Poly vinyl alcohol Fiber Aggregate Produced by an Electrospinning Method Journal of Polymer Science
16. NA S amp LIM C T 2004 Electrospinning and mechanical characterisation of gelatin nanofibers Polymer 45 5361 5368 JARUSUWANNAPOOM T HONGROJJANAWIWAT W JITJAICHAM S WANNATONG L NITHITANAKUL M PATTAMAPROM C KOOMBHONGSE P RANGKUPAN R amp SUPAPHOL P 2005 Effect of solvents on electro spinnability of polystyrene solutions and morphological appearance of resulting electrospun polystyrene fibers European Polymer Journal 41 409 421 JIANG H L ZHAO P C amp ZHU K J 2007 Fabrication and characterization of zein based nanofibrous scaffolds by an electrospinning method Macromolecular Bioscience 7 517 525 KESSICK R FENN J amp TEPPER G 2004 The use of AC potentials in electrospraying and electrospinning processes Polymer 45 2981 2984 KESSICK R amp TEPPER G 2004 Microscale polymeric helical structures produced by electrospinning Applied Physics Letters 84 4807 4809 KIDOAKI S KWON I K amp MATSUDA T 2005 Mesoscopic spatial designs of nano and microfiber meshes for tissue engineering matrix and scaffold based on newly devised multilayering and mixing electrospinning techniques Biomaterials 26 37 46 KIM C amp YANG K S 2003 Electrochemical properties of carbon nanofiber web as an electrode for supercapacitor prepared by electrospinning Applied Physics Letters 83 1216 1218 KO F GOGOTSI Y ALI A NAGUIB N YE H YANG G LI C amp
17. User Manual The electrospinning platforms ES1a and ES4 ES1a Page 1 0f 43 Page 2 of 43 Table of Contents Table of Cohen 3 1 Overview of the electrospinning platform 5 LE PuoseL 544 5 152 Principles ai eerie P ten mie el abe br eI e weak 5 te MANE RAR 6 1 4 Specia Sido pF CE EDD uio ne S de 6 2 1 Directions Of Use Lura 7 ea KEN EEE onte mum bet audits 8 3T Parto CMECKINSE NR 8 Bd Initial ASSO DW sis carts vie oi iae eda Na 9 3 2 1 The Assembly Test csisssescicisecascndnonisonsconsesuavevathormnenseranexanans 10 3 3 Places of the other elements needed for electrospibbilli enra E 10 9 4 Operations ur E een 11 3 9 MANE B cat n Ipae EC ER RN 14 TA 17 4 1 How do I make up a solution of PVOH 17 4 2 What can I use for a target rrarnnrnnnnnnrrnnnnnnrrrnnnnneene 17 4 3 Can I use a syringe pump rrranernranrrnnanrrnnnnernnnnsrnnnneee 17 4 4 What is the rate of deposition 17 Page 3 of 43 4 5 Why doesn t the machine need an enclosure to be clle 18 GONG 19 6 APPeNd see 23 Appendix How to specify a ventilation system when using hazardous solvents hausa 23 Appendix II Why doesn t the machine need an enclosure tO DE SALE m c 25 Appendix III Electrospinnable materials and conditions 27 Reier 37 Page 4 0f 43 1 Overview of the electrospinning platform 1 1 Purpose The aim
18. WILLIS P 2003 Electrospinning of Continuous Carbon Nanotube Filled Nanofiber Yarns Advanced Materials 15 1161 1165 KOSKI A YIM K amp SHIVKUMAR S 2004 Effect of molecular weight on fibrous PVA produced by electrospinning Materials Letters 58 493 497 LEE J S CHOI K H GHIM H D KIM S S CHUN D H KIM H Y amp LYOO W S 2004 Role of Molecular Weight of Atactic Poly vinyl alcohol PVA in the Structure and Properties of PVA Nanofabric Prepared by Electrospinning Journal of Applied Polymer Science 93 1638 1646 LEE S amp OBENDORF S K 2006 Developing protective textile materials as barriers to liquid penetration using melt electrospinning Journal of Applied Polymer Science 102 3430 3437 Page 39 of 43 LEE S J LIU J OH S H SOKER S ATALA A amp YOO J J 2008 Development of a composite vascular scaffolding system that withstands physiological vascular conditions Biomaterials 29 2891 2898 LI M GUO Y WEI Y MACDIARMID A G amp LELKES P I 2006 Electrospinning polyaniline contained gelatin nanofibers for tissue engineering applications Biomaterials 27 2705 2715 LYONS J LI C amp KO F 2004 Melt electrospinning part I processing parameters and geometric properties Polymer 45 7597 7603 MEGELSKI S STEPHENS J S CHASE D B amp RABOLT J F 2002 Micro and Nanostructured Surface Morphology on Electrospun Polymer Fibers M
19. acromolecules 35 8456 8466 MIYOSHI T TOYOHARA K amp MINEMATSU H 2005 Preparation of ultrafine fibrous zein membranes via electrospinning Polymer International 54 1187 1190 MOROZOV V N MOROZOVA T Y amp KALLENBACH N R 1998 Atomic force microscopy of structures produced by electrospraying polymer solutions nternational Journal of Mass Spectrometry 178 143 159 OHKAWA K CHA D KIM H NISHIDA A amp YAMAMOTO H 2004 Electrospinning of Chitosan Macromolecular Rapid Communications 25 1600 1605 POWELL H M amp BOYCE S T 2008 Fiber density of electrospun gelatin scaffolds regulates morphogenesis of dermal epidermal skin substitutes Journal of Biomedical Materials Research Part A 84A 1078 1086 QIN X H WAN Y Q HE J H ZHANG J YU J Y amp WANG S Y 2004 Effect of LiCl on electrospinning of PAN polymer solution theoretical analysis and experimental verification Polymer 45 6409 6413 QIN X H WANG S Y SANDRA T amp LUKAS D 2005 Effect of LiCl on the stability length of electrospinning jet by PAN polymer solution Materials Letters 59 3102 3105 QIN X H YANG E L LI N amp WANG S Y 2007 Effect of Different Salts on Electrospinning of Polyacrylonitrile PAN Polymer Solution Journal of Applied Polymer Science 103 3865 3870 RENEKER D H YARIN A L FONG H amp KOOMBHONGSE S 2000 Bending instability of electrically charge
20. cut to appropriate length to be use to be use 7 2 Glass Header tank 2 Glass Header tank 8 1 Toolbox containing 1 Toolbox containing 1x Allen key set 1x Allen key set 1x 10mm spanner 1x 10mm spanner 1x 11mm spanner 1x 11mm spanner r cm Electr Ospinz TEM Page 8 of 43 3 2 Initial Assembly A Unpack and check that the parts are all present B Remove the four machine screws and mount the target plane to the end of the spinning platform in the middle for ES4 do not over tighten the screws C D Plug the spinning platform lead into the back of the control box E Plug the power cable into the back of the control box and to the power supply Page 9 of 43 3 2 1 The Assembly Test F Check that the earthed power outlet has a good earth by plugging in the power lead with the switch OFF and checking for Voltage to another earthed point This check should be repeated each time the ES1a is used to keep the power supply G Turn on the power at the wall ensure that the HV Adj Knob is turned to Zero and turn on the ES1a the blue light on top of the control box should light up H Turn the HV Adjuster knob slowly to full power and back the meter should smoothly move between 0 and 33kV l Turn off the ES1a or the ES4 it is ready to use 3 3 Places of the other elements needed for electrospinning Header Earth M Page 10 of 43 3 4 Operation 1 Perform the previous as
21. d liquid jets of polymer solutions in electrospinning Journal of Applied Physics 87 4531 4547 Page 40 of 43 RISTOLAINEN N HEIKKILA P HARLIN A amp SEPPALA J 2006 Poly vinyl alcohol and polyamide 66 nanocomposites prepared by electrospinning Macromolecular Materials and Engineering 291 114 122 SAMATHAM R amp KIM K J 2006 Electric current as a control variable in the electrospinning process Polymer Engineering and Science 46 954 959 SELLING G W BISWAS A PATEL A WALLS D J DUNLAP C amp WEI Y 2007 Impact of solvent on electrospinning of zein and analysis of resulting fibers Macromolecular Chemistry and Physics 208 1002 1010 SELLING G W WOODS K K SESSA D amp BISWAS A 2008 Electrospun zein fibers using glutaraldehyde as the crosslinking reagent Effect of time and temperature Macromolecular Chemistry and Physics 209 1003 1011 SHAO C KIM H Y GONG J DING B LEE D R amp PARK S J 2003 Fiber mats of poly vinyl alcohol silica composite via electrospinning Materials Letters 57 1579 1584 SHENOY S L BATES W D FRISCH H L amp WNEK G E 20053 Role of chain entanglements on fiber formation during electrospinning of polymer solutions good solvent non specific polymer polymer interaction limit Polymer 46 3372 3384 SHENOY S L BATES W D amp WNEK G 2005b Correlations between electrospinnability and physical gelation P
22. d to be in contact with a live part of the machine for more than five hours 3 1 Minimum current required to produce Ventricular Fibrillation irrespective of voltage Pt 2x1073A2s I x 0 01s 2 x 1073A s 2 x 10 3A2s5 gt SS 0 01s I gt 0 4472A Note The EMCO high voltage power supply cannot supply more than 0 33mA or 0 33 x 10 A 2 There may be potential danger to those with a very weak heart or a pacemaker users who fall into either of these categories are advised to consult their doctor as to the likely risk in their particular case 3 For an impulse current Amps of short duration t lt 10ms through the body the principal factor for the initiation of ventricular fibrillation is the value of I x t Intensity x time or t IEC 2007 At high applied voltages the resistance of the adult body left hand to right hand is at least 575 ohms for 95 of the population IEC 2005 Note that the figures quoted for resistance are typical for a healthy adult and refer to the resistance measured through dry skin if the skin is punctured or wet then the resistance is reduced The IEC gives a threshold value of Specific Fibrillation Energy for a 1 ms current impulse of 2 x 10 A s Below this threshold there is no evidence of fibrillation The Specific Fibrillation Energy can be regarded as the energy dissipated per unit resistance of the body through which the current flows Note that specific here means p
23. er unit resistance rather than per unit mass Page 25 of 43 Time required producing Ventricular Fibrillation with EMCO supply I t 2 x 1073A s 0 33 x 1073A t 2 x 1073A s 2 x 103A s t 0033 x 1032 t 5 1hours References IEC 2007 IEC TS 60479 2 2007 Effects of human beings and livestock Part 2 Special aspects IEC 2005 IEC TS 60479 1 2005 Effects of human beings and livestock Part 1 General aspects Page 26 of 43 Appendix III Electrospinnable materials and conditions Solvents Water Acetone Megelski et al 2002 Chloroform Ethanol N N Dimethylformamide DMF Son et al 20049 0 5 M Acetic Acid Bhattarai et al 2005 Water Methanol 90 10 Kessick and Tepper 2004 Water Ethanol 60 40 Reneker et al 2000 Synthetic Polymers Polyethylene oxide PEO Typical Processing Parameters Concentration 10 Megelski et al 2002 Molecular Weight 400 000 Deitzel et al 2001a Voltage 10 kV 20 kV Son et al 2004a Distance 15 cm Deitzel et al 2001a Electric Field 0 5 kV cm 1 kV cm Shin et al 2001a Processing Parameters Range Conc 196 Doshi and Reneker 1995 1096 Deitzel et al 2001b My 300 000 Sun et al 2006 2 000 000 Shin et al 2001b Voltage 1 kV Sun et al 2006 30 kV Kidoaki et al 2005 Distance 5 cm Kidoaki et al 2005 40 cm Theron et al 2005
24. he metal frame of the ES1a or ES4 before touching any other part of the equipment gt Electrospun fibres are charged during manufacture this charge may be transferred to the depositing area This charge is very low and provided the user is earthed should be safe to handle gt After the equipment is turned off the high voltage system will take about 2 seconds to discharge do not touch the spinning bush during this time gt Donotuse this equipment unless the spinning tip and the feed hose are in place gt Always ensure that there are no volatile gases near the ES1a or ES4 during operation as the spark from a static discharge could cause ignition When using hazardous chemicals e Read the Material Safety Data Sheet of each hazardous products e f there is no other way to be safe use the personal protective equipment such as gloves respiratory masks protective glasses lab coat and shoes Page 7 of 43 3 General Guide 3 1 Parts checklist furnished with the spinning platform ES1a and ES4 Electrospinning platform ES1a Electrospinning platform ES4 ES1a ES4 1 1 ES1a spinning platform 1 ES4 spinning platform 2 1 ES1a Control Box 1 ES4 Control Box 3 1300x350mm Target plane with 4 1 300x350mm Target plane with 4 machine screws machine screws 4 1 Power cable 1 Power cable 5 1 Constant Head system 2 Constant Head system 6 2m Hose to be cut to appropriate length 2m Hose to be
25. in from fish skin International Journal of Biological Macromolecules 42 247 255 SPIVAK A F DZENIS Y A amp RENEKER D H 2000 A Model of Steady State Jet in the Electrospinning Process Mechanics Research Communications 27 37 42 SUN D CHANG C LI S amp LIN L 2006 Near Field Electrospinning Nano Letters 6 839 842 SUNDARAY B SUBRAMANIAN V NATARAJAN T S XIANG R Z CHANG C C amp FANN W S 2004 Electrospinning of continuous aligned polymer fibers Applied Physics Letters 84 1222 1224 SUTASINPROMPRAE J JITJAICHAM S NITHITANAKUL M MEECHAISUE C amp SUPAPHOL P 2006 Preparation and characterization of ultrafine electrospun polyacrylonitrile fibers and their subsequent pyrolysis to carbon fibers Polymer International 55 825 833 THERON S A YARIN A L ZUSSMAN E amp KROLL E 2005 Multiple jets in electrospinning experiment and modeling Polymer 46 2889 2899 THERON S A ZUSSMAN E amp YARIN A L 2004 Experimental investigation of the governing parameters in the electrospinning of polymer solutions Polymer 45 2017 2030 TUNGPRAPA S JANGCHUD I amp SUPAPHOL P 2007 Release characteristics of four model drugs from drug loaded electrospun cellulose acetate fiber mats Polymer 48 5030 5041 WANG C HSU C H amp LIN J H 2006a Scaling Laws in Electrospinning of Polystyrene Solutions Macromolecules 39 7662 7672 WANG H
26. jet is an expanding helix but this is commonly called the whipping instability Page 22 of 43 4 Appendix Appendix I How to specify a ventilation system when using hazardous solvents Some solvent and diluents systems used in electrospinning are hazardous by contact or inhalation To limit any hazards caused by the normal evaporation rate of the solvent to the atmosphere it is recommended to use a lid on the header tank usually a watch glass The Electrospinz machine is designed to fit inside standard laboratory fume cupboards This is the recommended method of limiting operator exposure to solvents fumes It may be necessary to switch off the fume cupboard ventilation during spinning to avoid the fibres being sucked away by the ventilation fan The fume cupboard door should therefore be kept closed during spinning The laboratory ventilation system should be checked if such solvents are used If you do not have access to a fume cupboard you should assess if the ventilation in your laboratory is adequate To do this you need to know the safe exposure limit of the solvent This can be found in the Material Safety Data sheet for the solvent It is also important to know the volume of the room where the electrospinning will occur As an example we will consider the use the Hexafluroisopropanol in a room with a volume of 140 m The exposure limit of this solution is 2 5 mg m so the limit will be reached when 3500 mg of solvent has e
27. latform keep the spinning bush and tip straight at a certain height aligned with the target An electric wire is inside making the contact between the high voltage supply and the metallic connector allowing the current to circulate Spinning Tip or Needle Spinneret A conic tube with a very small exit at the tip reducing considerably the flow of liquid allowing adjustments to the flow just by modifying the height of the header tank It is positioned at the tip of the metallic connector A micropipette tip or hypodermic syringe needle is often used Stable or continuous jets The stable part of the jet starts with a Taylor cone at the tip of the spinning needle To achieve this it is necessary to adjust the flow of liquid if it is too quick there will be a large droplet at the tip of the needle and the jet will not be continuous if it is too slow there will be a too small Taylor cone and the jet will not be continuous either It is also possible to modify the tension applied to the fluid to obtain the Taylor cone the higher the voltage will be the higher the fluid consumption and flow rate will be Straight Jet Axisymetric Jet The straight jet is a jet usually formed after the Taylor before it begins to whip This or those jet s is are more or less longer depending in the parameters the kind of solution used the distance between the needle tip and the collector the kind of collector and the applied voltage Surface tension The surface
28. made of polyethylene PE e Electrical connection fittings are made of brass e Header tank is made of borosilicate glass e Hose is made of Silicone rubber e Spinning tip is made of high density polypropylene Power Supply Single phase 100 to 240 VAC 1 amp maximum Power supply socket is a DIN standard fitting most computer cords will fit this Contact Electrospinz Limited 44 Lee Street Blenheim 7301 New Zealand Email sales electrospinz co nz Phone 64 3578 8092 Page 6 of 43 2 Safety 2 1 Directions of use High voltage power can present a serious risk of personal injury if not used in accordance with these safety instructions All users of this equipment must have read and understood the contents of this manual before operation is begun The ES1a and ES4 complies with the relevant New Zealand standards and has been constructed to comply with the electrical part of the BS EN 50 059 1991 specification for hand held spraying equipment for non flammable material for painting and finishing Although the output voltage can be as high as 33 000 Volts the maximum output current cannot exceed 0 3mA No conducting parts of the machine that are not earthed can be touched by the operator during normal operation provided that these instructions are correctly followed Caution Static charges may be present on insulated components even when the equipment is turned off gt Users MUST ALWAYS earth themselves by holding t
29. olymer 46 8990 9004 SHIN C CHASE G G amp RENEKER D H 2005 Recycled expanded polystyrene nanofibers applied in filter media Colloids and Surfaces A Physicochemical and Engineering Aspects 262 211 215 SHIN Y M HOHMAN M M BRENNER M P amp RUTLEDGE G C 20013 Electrospinning A whipping fluid jet generates submicron polymer fibers Applied Physics Letters 78 1149 1151 SHIN Y M HOHMAN M M BRENNER M P amp RUTLEDGE G C 2001b Experimental characterization of electrospinning the electrically forced jet and instabilities Polymer 42 9955 9967 SMIT E BUTTNER U amp SANDERSON R D 2005 Continuous yarns from Electrospun Fibers Polymer 46 2419 2423 SON W K HO YOUK J SEUNG LEE T amp PARK W H 2005 Effect of pH on electrospinning of poly vinyl alcohol Materials Letters 59 1571 1575 Page 41 of 43 SON W K YOUK J H LEE T S amp PARK W H 2004a The effects of solution properties and polyelectrolyte on electrospinning of ultrafine poly ethylene oxide fibers Polymer 45 2959 2966 SON W K YOUK J H LEE T S amp PARK W H 2004b Electrospinning of Ultrafine Cellulose Acetate Fibers Studies of a New Solvent System and Deacetylation of Ultrafine Cellulose Acetate Fibers Journal of Polymer Science Part B Polymer Physics 42 5 11 SONGCHOTIKUNPAN P TATTIYAKUL J amp SUPAPHOL P 2008 Extraction and electrospinning of gelat
30. onstant pressure feed header tank with a wide range of polymers and solvent but if you are working with an exceptionally viscous material a syringe pump may be the answer The pump can be connected through the spinning bush and pipette in the normal way What is the rate of deposition The rate is dependent on your choice of polymer system but will decline with time as the deposited fibre acts as an insulator and allows a charge to build up on the target The PVOH supplied will initially deposit at about 140ug s after about 10 minutes Page 17 of 43 Why doesn t the machine need an enclosure to be safe The Electrospinz machines are designed to have an intrinsic low capacitance This is achieved by minimising the amount of metal surfaces that are charged by the power supply and the bonding to earth of all the metal surfaces of the machine Good bond continuity is ensured by welding the component parts of the structure together These design principles result in a machine capacitance of less than 10pF Surrounding the machine with an insulating cabinet would increase the capacitance of the system Low machine capacitance is an important safety feature for the following reasons When the machine capacitance gt 10pF is considered in connection with a human body resistance of approximately 500 ohms IEC 2005 this means the capacitive charge will discharge in under a millisecond leaving only the continuous supply capacity of the power
31. pecial parts can be ordered from Electrospinz Limited Page 14 of 43 Circuit Diagram Any servicing of the electrical system must be done by a qualified person in accordance with local requirements Wire numbers shown are for the Plug socket multi core cable and HV power supply 100 to 240 VAC Omron 24VDC Power supply Green Yellow Blue Indicator Light ai EMCO 4330 HV Power Supply Panel Meter 0 10 VDC Scaled 0 33 KV Circuit Diagram for ES1a Electrospinning Platform Page 15 of 43 Blue Indicator Light EMCO 4330 HV Power Supply Panel Meter 0 10 VDC Scaled 0 33 KV Blue Indicator Light EMCO 4330N HV Power Supply Panel Meter 0 10 VDC Scaled 0 33 KV HV Adj 4K7ohm Circuit Diagram for ES4 Electrospinning Platform Page 16 of 43 FAQ How do I make up a solution of PVOH Polyvinyl Alcohol PVOH is soluble in water but you should heat the distilled water to 60 C and the powdered polymer 7 8wt should be stirred in very gradually to avoid the formation of lumps What can I use for a target Domestic aluminium foil works very well and sets of identified sample plates are available Handle with gloves to avoid the transfer of grease and moisture from your hands The target will need to be connected to earth through any part of electrospinner chassis or the earth stud Can I use a syringe pump If you wish the Electrospinz platform works by the c
32. pinning jet Photo by R Lamberts PFR Page 5 0f 43 1 3 Warnings This is a research machine designed to allow maximum access to the process for research purposes The only pieces that are significantly live during operation are the pipette tip the transfer pipe and liquid within the reservoir The electrospinning machine runs at between 0 33 000 volts the maximum current delivered by the machine is 0 3mA a level of current much lower than that required for injuring a human However a shock from the machine is disagreeable like a shock from static discharge 1 4 Specifications Description The ES1a and ES4 are designed to be used by competent operators in a laboratory environment using an aqueous solution Other solutions may be spun but the materials of the header tank hose and spinning tip may need to be changed or adapted The ES1a and ES4 is a one or two part machine with a solid easy to clean base The constant head system is adjustable and has both coarse and fine adjustment The moveable spinning head can be set from zero to 150mm for the ES1 and from zero to 200mm for the ES4 from the fixed target plane this can be adjusted during operation The power to the spinning head is adjustable from zero to or 33 000 VDC from the separate control box Materials e Base and Control Box are constructed from stainless steel e Insulating materials are made of Polyoxymethylene POM e Target plane 300mm x 350mm x 10mm is
33. rospraying the operation of creating droplets with a nano size through a similar process used for electrospinning Feed Pipe Silicone Pipe Feed Hose a plastic hose used to connect the reservoir to the spinning tip via the metallic spinning bush Flow Rate Mass Flow Rate The flow speed of the liquid effectively the spinning speed of the process Page 19 of 43 Fluid Pressure Pressure applied to the fluid to regulate the flow and therefore stabilize the electrospinning process This can be controlled in increasing or decreasing the height of the Header Tank Grounded Collector Target Substrate Grounded Electrode the object used to collect the fibres it may different shapes according to the kind of fibres wanted a simple metallic plate or aluminium foil results in the creation of random fibres but a metallic wire frame results in the creation of aligned fibres This collector must be connected to the earth to avoid charge accumulation High Voltage Electric Current The electric current that circulates between the spinning tip and the grounded collector The maximum current which can be produced is under 0 33 mA See FAQ Why doesn t the machine need an enclosure to be safe Mass Deposition Rate The mass of fibres produced within a certain amount of time Magnetisation While using a metallic plate as a collector using a magnet to keep the plate vertical will be useful However during the process the plate will acquire a ce
34. rtain magnetisation that may interfere with the weighing process and misrepresents the real amount of fibres which have been deposited on the plate Using a demagnetizer after electrospinning can prevent interferences while weighing the plate This effect is only noticeable when using a 4 figure balance Nanofibres Fibres which diameter of less than 100 nanometres Porous surface and smooth fibres Nanofibres can have varying surface s morphologies for example the fibre surface may be pitted or smooth Removable Spinning Bush Metallic Connector This element makes the connexion between the silicone hose and the spinning tip It is connected to the high voltage supply Reservoir Header Tank contains a certain amount of liquid and by varying the height of the reservoir controls the pressure or head of the flowing liquid SEM Scanning Electron Microscope A type of electron microscope that produces images of a sample by scanning it with a focused beam of electrons The electrons interact with atoms in the sample producing various signals that can be detected and that contain information about the sample s surface topography and Page 20 of 43 composition The electron beam is generally scanned in a raster scan pattern and the beam s position is combined with the detected signal to produce an image SEM can achieve resolution better than 1 nanometre Spinning Post or Electrode High Voltage Electrode This part of the electrospinning p
35. sembly test F to I 2 Place the glass header tank between the tongs of the constant head system 3 Insert the spinning bush at the top of the spinning post 4 Connect the hose from the header tank to the spinning bush 5 Insert the spinning tip over the spigot on the other side of the spinning bush 6 Place a collector on the target such as an aluminium foil or a metallic plate 7 Earth the target area connect the target to the ES1a or ES4 metallic platform If this is not done then the fibres will be drawn to the nearest earthed thing This is not necessarily the ES1a or ES4 it may be any structure within reach Page 11 of 43 8 Pour the prepared polymer into the header tank 9 Raise the header tank to allow the liquid to flow to the tip of the spinning needle with the course or manually 10 Maintain the header tank to hold a small droplet of polymer at the spinning tip A piece of paper towel may be placed on the ES1a or ES4 bed between the spinning tip and the target plane to assist with cleaning 11 When the polymer is seen to be almost at the spinning tip lower the header tank to provide a head of about 15mm above the spinning tip This will need to be adjusted once spinning has begun Page 12 of 43 12 With the HV Adj knob turned to zero turn on the switch While watching closely to the tip of the electrospinning needle raise the voltage until the Taylor cone appears this is normally visible with
36. tension of a liquid is an important parameter while doing electrospinning It is a contractive tendency of the surface of a liquid that allows it to resist an external force This property is caused by cohesion of similar molecules and is responsible for certain of liquids properties Therefore it is a useful parameter to know while creating solutions for electrospinning Surface tension has the dimension of force per unit length or of energy per unit area Taylor Cone The cone observed at the tip of the spinning needle when high voltage is applied to the liquid it is apparent as a deformation at the end of the liquid meniscus at the spinning tip The apex of the cone is the point of ejection of the liquid stream what forms the jet The cone is named after Sir Geoffroy Ingram Taylor 1886 1975 who first described it Page 21 of 43 TCD Tip to Collector Distance It s the distance between the spinning tip and the grounded collector a typical TCD used for electrospinning is 10 cm Uniform fibres fibres are uniform when they have the same characteristics diameter alignment and morphology Whipping or Bending Instability Whipping Envelope During its flight the jet is drying out and at a variable distance from the needle the jet starts to whip and bend until it arrives at the collector At its arrival the jet is ideally only composed by the polymer the solvent has all been lost in flight Strictly speaking the flight path of the
37. vaporated 140 m 2 5mg m What we need to know next is the amount of time necessary to reach that limit for that purpose we can use the evaporation rate of PVOH in water which is 60 mg h during electrospinning Then we can calculate the amount of time to reach the limit _ 350mg 5 83 h 5h49 min 48s 60 mg h But this evaporation rate is true only for the PVOH so we must apply safety coefficients to that calculation x5 or x10 are a safe allowance Page 23 of 43 With an evaporation rate multiplied by 5 we find this result 350 tio gt 1 17h 1h10 min 60 x 10 With an evaporation rate of 10 we find this result t zo 0 58h 35 mi bays 35 min Those times means that the room air would need to be completely renewed within 1h or 35 minutes depending on the safety level required Depending on the hazards and the amount of product used it would be better to apply the safety rating of 5 or 10 Even if the spinning platform is completely isolated it is strongly recommended to always wear a respirator when using these kinds of hazardous chemicals Page 24 of 43 Appendix II Why doesn t the machine need an enclosure to be safe An Electrospinz machine at maximum current output short circuit conditions cannot produce enough current to disrupt the action of the heart 1 It can be calculated that for the supply to produce enough energy to disrupt the activity of the heart the victim 2 would nee
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