Characterizing Hydrogel Imposed Strain Fields on Brain Tissue Phantom for Use in Neural Implant Device Coatings in Presence of Micromotion By Maxwell Ethan Plaut Submitted to the Department of Materials Science and Engineering in Partial Fulfillment of the Requirements for the Degree of Bachelor of Science at the Massachusetts Institute of Technology MASSACHUSETTS INSTITUTE OF TECHNOLOGY JUN 0 June 2014 14 LIBRARIES ©2014 Maxwell Plaut All rights reserved The author hereby grants to MIT permission to reproduce and to distribute publicly paper and electronic copies of this thesis document in whole or in part in any medium now known or hereafter created. Signature of Aut hor Signature redacted Department of Materials Science and Engineering 9,2014 4 ,May ool Certified by Signature redacted Dai H. Koc Prfso ofEgnern Michael Cima V David H. Koch Professor of Engineering Thesis Supervisor Accepted by Signature redacted f IVV/ Jeffrey Grossman Associate Pofessor of Materials Science and Engineering Chairman, Undergraduate Committee Characterizing Hydrogel Imposed Strain Fields on Brain Tissue Phantom for Use in Neural Implant Device Coatings in Presence of Micromotion By Maxwell E. Plaut Submitted to the Department of Materials Science and Engineering on May 9, 2014 in Partial Fulfillment of the Requirements for the Degree of Bachelor of Science in Materials Science and Engineering ABSTRACT Glial scar tissue forms in the brain as a response to the implant injury and hampers the effectiveness of the implant treatment. Constant relative micromotion between the mechanically mismatched neural implant and brain tissue is thought to play a key role glial scar formation. This study investigated the effects of poly(ethylene glycol) (PEG) hydrogel coatings for glass brain implant devices on strain fields imposed by those devices to brain tissue due to micromotion in the brain. PEG hydrogels were created using macromers of 2000-8000 M, and 5-20 wt.% in solution. The moduli of the hydrogels were calculated via Hertzian analysis of force-deflection curves produced using an AFM tip as a nanoindenter. The moduli of the samples did not change significantly with change in macromer M., but did change with solution concentration. 20% gels had moduli of 120-180 kPa and 5-10% gels had moduli of 0-20 kPa. The strains imposed by the coated devices were found to be lower at the surface by ~30% as compared to uncoated and the strain field dropped off much more quickly. 2 Introduction Many neurological diseases, termed circuit disorders, are the result of errors in communication between anatomically distinct regions of the brain which make up a neural circuit' 2 . Circuit disorders can be severely debilitating to the persons with them and some, such as anxiety and depression, are rather prevalent today. Some of these disorders have been shown to be associated with activity at particular foci within the brain . While the understanding of these diseases, and how they affect brain function has increased tremendously in recent times, there is a lack of technology that enables effective treatment of these disorders. Treatments containing direct electrical stimulation to the specific foci in the brain have shown that targeted treatment at the neural circuit level can be effective at treating these disorders 34,6 ''. Members of the Cima lab have developed a novel drug delivery implant device, named the injectrode, which is capable of electrically stimulating and recording specific neural areas with an electrode while simultaneously delivering nanoliter volumes of drug solutions on demand to targeted regions of the brain through a borosilicate capillary. This targeted approach is expected to be more effective in regulating circuit activity than electrical stimulation or drug delivery alone. There are several materials issues associated with the use of a chronic drug delivery device within the central nervous system (CNS). Glial scar tissue forms in the brain as a response to the implant injury and hampers the effectiveness of the implant treatment7. Many current implant devices and treatment efforts result in significant glial scarring around the implant device-. Glial scarring has an increased impendence as compared to normal brain tissue, and since many of these treatments include electrical stimulation or 3 recording via implanted electrode, the devices' effectiveness tends towards being negligible over time'". Damage resulting from micromotion between the brain tissue and implant is thought to be a key contributor to glial scar formation . Experimental attempts to reduce glial scar formation from a materials approach have shown modest success, but have made use of materials with moduli that are still several orders of magnitude higher than that of brain tissue '14 Hydrogels are highly swollen cross-linked polymer networks widely used in biomedical applications due to their similar mechanical properties to biological tissue 5 1' 6 Hydrogel coatings that incorporate conductive polymers have been used to improve the recording capabilities of neural probes ' 1 . However, the effect that the mechanical properties of these coatings have on the chronic glial scar response has not been extensively characterized. The aim of this project will investigate the use of hydrogel coatings (100 [tm scale), with moduli on the order of brain tissue, to reduce the strain field resulting from implantation. The results of these experiments will help guide the design of future neural implants and will serve as a crucial step towards the implementation of chronic delivery systems to treat neurologic diseases of the brain. Theory Glial Scarring. In order to effectively treat circuit disorders, devices such as the injectrode require chronic operation. The injectrode must also operate safely and effectively at the time of implantation and continue to do so in the presence of bodily biological response to the device. The brain's primary immune to response to neural 4 electrodes, astrogliosis, results in the formation of glial scar tissue around the electrodes. The main cellular contributors in the astrogliosis response to implants or other injury to the central nervous system are astrocytes and microglia. Astrocytes, characterized by immunostaining for the intermediate filament protein glial fibrillary acidic protein (GFAP)19 , are the main component of glial scar tissue. Microglia are macrophages in the brain that engulf particles and secrete proteins that affect a variety of processes that support inflammation. Astrogliosis is generally divided into two main phases, the acute phase and the chronic phase7 . Prolonged Reactive Response Ealy Reactive Response (A) Possible snn Possile signling patways pabWays Possibl, cell banstounasons PossibleOcll tanstonnatons (B) Figure 1. Possible mechanics of cellular response to an implant. Acute phase (a) and chronic phase (b) of cellular response to implant device injury. Neurons are in pink, microglia in blue, vasculature in purple and astrocytes in red.7 The short-term response to foreign object implantation in the central nervous system is what is referred to as the acute response. The acute response occurs over about the first two weeks of implantation and is characterized by a large amount of microglia activity. Implantation of the device causes injury to the brain through cell damage, blood vessel severing and disruption of the extracellular matrix. This injury causes the release of several protein factors into the area to promote inflammation and clotting20 . The proteins promoting inflammation cause inflammatory cells and microglia to join and form an 5 envelope of cells around the injury. The microglia then breakdown red blood cells in the area and any cellular remains from the injury, then release cytokines and reactive oxygen intermediates in order to promote inflammation. This inflammatory response can negatively affect device effectiveness in the area of the injury7 . Implantation times longer than two weeks usually mark the end of the acute phase and lead to the chronic phase of the astrogliosis. The chronic phase is characterized by the formation and densification of glial scar tissue. Astrocytes isolate the injury site from the rest of the neural tissue even further than was done in the acute phase and increase production of certain extracellular molecules, including chondroitin sulfate proteoglycans, that inhibit axon regeneration 7,21,22. The glial tissue, typically a few hundred microns thick, reaches its full size 4-6 weeks after the initial injury and remains generally stable for the duration of the implantation (Figure 2)1o,23 2 WAeks 6 Wanks 4 Wmeek 12 WeekR Figure 2 Time course of glial scar formation around a neural implant. Image was made by GFAP immunostaining. At 2 and 4 weeks the glial scar falls back into void left by the electrode. At 6 and 12 weeks the glial scar is a dense sheath which does not collapse into the void2 1 This process of the chronic phase is analogous to the fibrous encapsulation observed around implants in other parts of the body 24-26. Additionally, microglia typically remain at the surface of the implant injury throughout the chronic phase forming a dense layer of cells on the implant surface that is surrounded by the glial scar 27 6 Glial scar is formed with the intent to protect the brain and the rest of the central nervous system from the implanted foreign body within the tissue as well as the reactive proteins and molecules released to the injury site in the process7,28,29. However, while generally beneficial, glial scar formation is believed to be a key contributor to implant device and electrode failure. Nearly half of recording electrode implants fail 6 months ". Neurons typically need to be after implantation despite initially operating properly 11,12 less than 100tm from the recording electrode to be recorded3 0 , and the formation of glial scarring forces neurons near the implant away from the injury site, decreasing the potential signal that can be recorded by these devices and eventually leading to complete failure of the electrode implant 26 . Glial scarring increases the impedance of the tissue, thus reducing the volume of tissue activated by electrical stimulation by up to 50%". This can be partially overcome to get the desired therapeutic effect on a given neural circuit through use of a higher current but a higher current can lead to neuron damage31. Sykova, et al. used ion selective electrode measurements to investigate how diffusion properties of cells change following astrogliosis in response to a stab wound 21,323, 3 and it was found that the astrogliosis leads to an increase in tortuosity, increase in the volume fraction of extracellular space, and decreased cellular uptake. This hindered diffusion environment likely affects the extra synaptic transmission of neurons, hinders diffusion of glucose and oxygen to cells from circulation, and contributes to the barrier to axon regeneration around the injury. It should be noted that the glial scar resulting from stab wounds should have slightly different properties than those resulting from chronic implants due to constant presence of brain micromotion in the case of chronic implants. 7 There have been many studies conducted with the goal of reducing the scarring response to implanted electrodes with results of varying success' 35'36 . These studies provide insight into the mechanisms of scar formation, and provide suggestions regarding device properties that are important to consider when designing chronic neural implants. One contributor, mechanical mismatch, will be a focus of this project and is discussed below. Modulus Mismatch and Micromotion. Brain tissue is constantly undergoing micromotions up to 40 pm in magnitude in rats due to respiration, vascular pulses, and rotational accelerations37,38 . Typical neural implant device materials have moduli that are many orders of magnitude higher than that of brain tissue. Constant relative motion between the neural implant and tissue is thought to play a key role in the chronic tissue Table 1. Moduli of common implant materials 49' 50 and brain tissue 4 1 response through constant aggravation of local inflammatory cells and damage to local vasculature 39 . This theory is supported by the finding that implants that are tethered to the skull result in a much greater glial scar response than Elastic MaterialModulus Material (GPa) 69 Borosilicate Glass Gold 80 200 Silicon Titanium 107 Polyimide Brain 2 .000005 untethered implants which are free to move with the brain's micromotion 4. Tethered implants are fixed in place relative to the skull and thus result in a greater relative motion between the implant and tissue. This results in greater injury and aggravation of tissue surrounding the implant and more extensive scar formation. Finite element analysis simulations have been conducted to investigate the effect that micromotion and mechanical mismatch have on the surrounding tissue' 41 . These simulations estimate the 8 amount of strain that the brain tissue experiences as a result of brain micromotion in the presence of neural implants of various mechanical properties. It was found that a probe composed of a hypothetical soft material with Young's modulus of 6MPa results in a strain two orders of magnitude less than that of a silicon probe with a modulus 200GPa41 . Poor tissue-device adhesion also was found to contribute to elevated strains. A tangential tethering force from tissue adhesion to the device reduced strains near the tip of the electrode by 94%41. This further corroborates the theory that tissue aggravation causes glial scar formation. Neural implant designs could incorporate materials with lower mechanical strengths or coatings that promote adhesion with neural tissue to reduce the extent of glial scar formation. Hydrogel Coating. It would follow, therefore, that implanting devices with a hydrogel coating would result in a reduced reactive gliosis response compared to uncoated glass devices following micromotion. Hydrogels are already widely used in biological applications and have mechanical properties similar to that of brain tissue15 16 . Although the presence of a hydrogel coating would likely not completely prevent scar formation due to the central nervous system's foreign body response, a mechanically matched coating would reduce injury to the brain tissue due to micromotion caused strain. This decrease in strain imposed on the brain would reduce the astrogliosis response and the overall size of the glial scar would be expected to be reduced, increasing the effectiveness of the device. Hydrogel Mechanics. The key properties in considering a hydrogel coating for a neural implant device are its mechanical properties. Due to the numerous controllable variables associated with the gel formation process, it is possible to tune to the mechanical 9 properties of the formed gel to match that of brain tissue, which has a modulus of-5kPa. The parameters that are controllable include the molecular weight of the gel precursor polymer chains and the concentration of those monomers in solution. The microstructural origin of gel elastic response is the entropic spring effect. Stretching polymer chains, or otherwise mechanically forcing them out of a high-entropy coil conformation, reduces the number of available microstructural conformations available to that chain, decreasing the entropy of the system. Since the potential entropic contribution to the free energy of the chains is so high, the stretched state is thermodynamically unfavorable. When the external stretching force is removed from the system the polymer chain will snap back to its equilibrium, unstretched state. Hydrogels are formed by linking together many smaller chains of a water-soluble polymer. One methods of crosslinking these chains is through radiation crosslinking using ultraviolet light. Irradiation of polymer containing solution causes the creation of free radicals which recombine to form chemical crosslinks between chains. The resulting gel can then swell in the presence of a solvent, which in the case of hydrogels, is water. The Young's modulus of these gels is highly dependent on the total crosslink density which includes both chemical and physical crosslinks. Increasing the crosslink density restricts chain movement within the network. As a consequence, this prevents deformation of the overall structure in response to applied stress. Crosslinking density is primarily tunable through selection of gel precursor. Free radical formation, the first step in chemical crosslinking, occurs at the ends of polymer chains. Increasing the density of polymer chains ends before gelation would therefore increase the resulting chemical crosslink density. The simplest way of increasing chain 10 ends is using small molecular weight chains as a precursor. Smaller molecular weight means fewer monomers per chains and a shorter chain, meaning an increase in chain ends per monomer. Figure 3 shows two different gels, one formed from high molecular weight chains and one formed from low molecular weight chains. a) b) Figure 3. Schematic of ideal networks. Schematic shows the difference in number of crosslinks, circled in red, between network polymers (in green) formed from high molecular weight polymeric chains (a) and low molecular weight chains (b). The chemical crosslink density is much higher in the low molecular weight case. This diagram does not take physical crosslinks into account Physical crosslinks occur when the polymer chains get entangled and restrict movement This is purely a topological constraint imposed on the system when two polymer chain intertwine and are relatively fixed in place by steric effects42 . These entanglement effects begin to occur at low chain length and have rather significant effects on the mechanical properties of the bulk polymer. Even in melt form, due to increasing entanglement, the viscosity of a polymer is related to the cube of the molecular weight 42. At longer chain lengths (>100 monomers) this entanglement effect is often the dominant crosslinking effect, especially at only small variations in degree of chemical crosslinking. 11 F V p - py f 4ha Win y s Figure 4. An entangled polymer chain forming physical crosslinks Gel modulus can also be affected by the polymer concentration in solution prior to crosslinking. Gelation procedures typically dictate that gels form from specific volume of solution, usually to obtain a particular thickness of shape of the gel. Under this condition, changing the concentration of polymer in the solution results in a change in total amount of polymer in the network while the volume of the total gel remains unchanged. Since solvent occupies the volume of gel not occupied by polymer, decreasing the polymer amount effectively increases the volume of solvent. This loss of connectivity allows the structure to yield more under applied stresses, meaning a lower modulus for those structures. Materials and Methods Materials. Poly(ethylene glycol) (PEG) (Mw~ 2000 - 8000 g/mol), methacrylic anhydride, 2-isocyanatoethyl methacrylate (IEM), ethyl ether, and triethylamine (TEA) were purchased from Sigma-Aldrich and used as received. Dichloromethane, sulfuric acid, hydrogen peroxide solution, 3-(Trichlorosilyl)propyl methacrylate (TPM), 2- 12 hydroxy-4'-(2-hydroxyethoxy)-2-methylpropiophenone, 2,2-dimethoxy-2phenylacetophenone and carbon tetrachloride were purchased from Sigma-Aldrich. Heptane was purchased from Macron Fine Chemicals and used as received. The glass slides used were 12mm diameter with a thickness of .1 6-.19mm and were purchased from Electron Microscopy Sciences. Glass capillaries were purchased from VWR. Fluorescent polystyrene particles with a diameter of 5.9ptm were purchased from Polysciences, Inc. and used as received. Equipment. The Cure Spot 50 from ADAC systems controlled the ultraviolet radiation source during gelation. Strain field measurements were performed using a standard bright field optical microscope from Micro-Tech Optical, Inc. Force and modulus measurements were taken using an atomic force microscope from Veeco, the Nanoscope IV with Multimode and Picoforce PEG Synthesis. Poly(ethylene glycol) dimethacrylate was prepared by the procedure described by Gibson et a, 43 . PEGDM was formed from the reaction of various PEGs, MA and IEM. An example of the synthesis of a 5k PEGDM is as follows. PEG (5 g, Z0.001 mol), 2.2 equiv of MA (0.34 g, 0.0022 mol), and TEA (0.2 mL) were reacted in =15 mL of dichloromethane over freshly activated molecular sieves (Z3 g) for 4 days at room temperature. The solution was filtered over alumina and precipitated into ethyl ether. The 43 product was filtered and then dried in a vacuum oven overnight at room temperature 0 0 H 0 N 0 00 0 , N 0 Figure 5. Structure of Poly(ethylene glycol) dimethacrylate 13 Surface Functionalization. Glass substrates were functionalized using standard protocols for surface modification as described by Revzin et al. 44' 45 . Substrates were cleaned in a 3:1 sulfuric acid:hydrogen peroxide "piranha" solution and then treated with TPM in a 1mM solution of 4:1 heptane:carbon tetrachloride in a nitrogen atmosphere. The substrates were washed and dried after each step. This treatment forms a monolayer of methacrylate groups on the surface on the glass to provide points for the PEG to covalently bond to the surface to prevent delamination 44 0 / OH OH OH Si0 SiI Si 0 0 0 I OH OH Si SiN I 0 0 _ _ I HO-Si TPM in 4:1 Heptane:CC 4 OH 0 -0 0 0 Si-OH LH 19 S,lo a OH 10101 I~ II Figure 6. Surface functionalization of glass substrates. A clean glass surface (left) gets functionalized to have methacrylate groups (rights) for PEG to bind to by TPM in a 4:1 Heptane:CCl 4 environment. Gel Formation. Functionalized glass substrates were then coated with a solution containing dissolved PEG macromers at the concentrations of 5,10 and 20% by weight, with .5% photoinitiator. Samples were coated via either a tube filling process, for capillaries, or direct pipetting onto the surface. The solutions were exposed to 365 nm ultraviolet radiation for to crosslink the PEG via free radical polymerization. The solution was exposed to UV for 90 seconds or, in the case of low concentrations, until gelation occurred for direct pipetting. The glass capillaries were suspended inside a larger glass tube for tube filling and solution was dripped into the tube and then pulled across the 14 surface of the capillary through capillary action. This method was utilized to ensure a uniform thickness of the hydrogel coating across and around the device. b Photoinitiator Light Figure 7. Schematic representation of the PEGDM network showing (a) cross-linked PEG chains and network defects including, (b) unreacted acrylate terminuses, (c) PEG cycles and (d) chain entanglements. Shaded arrow shapes represent reacted acrylates, unshaded arrow shapes represent unreacted acrylate, and dark lines represent PEG chains esterified to the acrylic acid. For clarity, short acrylate chains are shown, but in actual gels these chain lengths may be much longer 6 . Force Measurements and Modulus Calculations. The atomic force microscope (AFM) is well suited for probing the local elasticity of small very soft samples 47 when the cantilver tip is used as a nanoindenter. Samples with swollen PEG hydrogel were placed in the AFM and probed by a spherical polystyrene tip with a diameter of 45plm and a cantilever spring constant of 14 N/m. Tip deflection as a function of depth of indentation was measured. The Young's moduli of the gels were then determined via Hertzian analysis of the resulting force-displacement curves. This analysis assumes that the hydrogels are deforming in a linear elastic fashion and there is negligible adhesion between the gels and the AFM tip. Using the methods presented by Lin et al., an AFM 15 was used to measure the relationship between tip deflection and depth of indentation into the gel. The force applied by the tip was calculated by F = kc(d - do) (1) where kc is the spring constant of the cantilever, d is the measured deflection, and do is the deflection offset at the point of contact 4 7. Using the spherical geometry of the tip it was then possible to derive the modulus from the relationship 1 F 4 E R22 3(1-V ) z - Zo) - (d - do)] 3/2 (2) where z is the measured translation of the cantilever, z is the translation of the cantilever at the contact point, R is the radius of the tip, v is the Poisson's ratio, which was assumed to be .5, and E is the Young's modulus47 . quad photodiode laser cantilever-tip sample Figure 8. Basic schematic of AFM. An AFM tip can be used as a nanoindenter n the sample and the force required to indent a sample can be calculated by measuring the deflection of the cantilever. 16 Particle Tracking Analysis. The brain undergoes micromotion in the radial directions (along device axis) due to vascular (1-3 pm) and respiratory pulsations (2-40 ptm) 37'38 . Agarose gel with fluorescent particles suspended was formed around the coated device to prevent shearing during insertion. The device was then displaced 20-40 Pm in the radial direction to simulate micromotion. Figure 9. Strain field measurement setup. The coated glass capillary (a) is immersed in agarose gel in a petri dish (b) under the optical microscope. It is held by a capillary holder (c) which is connected to a stepper motor capable of simulating micromotion in the brain in the radial direction Bright field images before and after deformation were analyzed to obtain the resulting displacements for each particle. The strain fields in the gel were calculated from the observed particle displacements using the particle image velocimetry plugin for ImageJ. Strain fields imposed by different samples were compared by examination of the 17 maximum particle displacement around the implant as well the variation displacement vectors as a function of distance from the implant 8 . This analysis determined the effect that hydrogel coatings have on cells directly around the implant, as well as estimate the volume of brain tissue around the implant that experiences stress resulting from micromotion respectively. Figure 10. Optical bright field microscope image of uncoated device. The black capillary is the uncoated glass device. The device is surrounded by agarose gel and the multitudes of black spots in the image are the polystyrene particles suspended in the gel used for strain field analysis. Results and Discussion Modulus Calculations of Gels. The moduli were visualized by plotting as a function of both molecular weight of the original chains of PEG and by the concentration of the polymer in the gel precursor solution. When comparing the moduli of the samples as a function of molecular weight of the original chains (figure 11), it seems as though varying the molecular weight of the polymer has little to no effect on the resulting modulus. Increasing the molecular weight 18 increased the resulting physical crosslink density slightly, but greatly decreased the chemical crosslink density. A great decrease in chemical crosslink density, without any physical crosslinking would result in a great decrease in modulus. In these samples, however, the degree of physical crosslinking seems to be the dominant factor in determining the modulus of the samples. The change in chemical crosslink density, modulated through the change in molecular weight, at least on this scale, has no significant effect on the modulus of samples of similar precursor solution concentration. Changing the concentration of PEG in the precursor solution does seem to be able to have a large effect on modulus of the samples. The modulus of the gel was observed to increase as a function of polymer concentration for all chain lengths (figure 12). This suggests a greater crosslink density at higher polymer concentrations. The 10% gels have slightly higher moduli than the 5% gels, but the set of 20% gels has considerably higher moduli than the other gels. This is likely due to the lower concentration polymer being too disperse in solution to form a homogenous distribution of clusters. This results in large defects in matrix, and reduced crosslinking, and thus a reduced modulus. At low concentration it is also more likely that the reactive terminuses of a single PEG chain react with themselves, further reducing the connectivity of the resulting gel. Somewhere in the range between 10%-20% a critical concentration is reached at which homogeneity is reached and the gel can properly form. 19 Modulus vs. Mw of PEG 200 180 y = -0.0056x + 178.39 160 140 +20Wt.% 120 *5Wt.% A 100 Wt.% 10 60 401 0 0009 y=- . rR 20 x + 18.172 = 0 84463 Sy 0 =- 0 2000 1000 3000 4000 Mw of PEG 5000 6000 7000 0 0 0 07 . x + 7. 3584 R=0.95922 - -- 8000 9000 (g/mot) Figure 11. Plot of modulus vs. molecular weight. Plot shows the change in modulus of samples using 5 wt.% (red), 10 wt.% (green) and 20 wt.% (blue) precursor solutions. For each concentration the modulus seems to change very little in response to changing molecular weight Modulus vs. Wt. % Polymer In Solution 200 150 2000 --.-, 4000 .8000 100 50.-- 0 5% 10% 20% PEG Conc In Sorn (Wt. %) Figure 12. Plot of modulus vs. concentration of PEG. Plot shows the change in modulus as a function of polymer concentration in precursor solution for given molecular weights on original polymer chains. There seems to be a threshold at which the modulus increases dramatically somewhere between 10%-20%. 20 Strain Field Analysis. The particle displacement vector fields were visualized by determining the movement of each polystyrene bead in the gel near the device tip after simulating micromotion through movement of the device and then plotting that movement as a vector. Cross sections of the vector plots were taken near the device tips and graphed showing the change in vector magnitude as a function of distance from the device. The strain imposed on the gel was highest right near the devices and decreased with distance from the device on all sides. Both the particle displacement at the surface of the device and the displacement at longer distances were smaller when the devices had a PEG coating as compared to the control. The polystyrene beads near the surface of the device in the uncoated sample move about 3Optm, which is the amount of movement applied to the device to simulate the micromotion. Near the surface of the hydrogel coated devices, which have a reduced modulus, the beads were found to move 15-20pm. The displacements in the coated device samples also have a higher rate of decrease as a function of distance from the device than the uncoated devices. The exception to this was the coated sample made from PEG-2000. The particle displacement on one side of the device was comparable to the particle displacement of the uncoated, while the other side has displacement more similar to the coated device (figure 13). This can be understood by looking at a picture of the device. The device has a hydrogel coating on one side, while the other side is essentially uncoated. This further corroborates the difference between imposed displacement fields from uncoated and coated devices. These finding also support those of the simulations 21 run by Jeyakumar et al. that soft materials imposed lower strain on brain tissue 43 undergoing micromotion than materials with high moduli . Figure 13. PEG-2000 coated device. The black part of the device is the glass capillary and the area below it is the PEG coating. There is very little coating above the device leading to strain behavior in that region more similar to that of uncoated devices. The red line denotes the line on which the cross section of the displacement field was taken. 25404 0004MW 200OMw C(0ntro4 - . - - - : 25M " "40 ' - - - I I 2000 200 4,500M 4000 -A 0 560 10M0 15011 2440 25M4 0 [5M0' 50 ll ,-" 6 "'P) 2000 2 0 500' 400 1506 '-i-44~4 2000 2500 (PM) Figure 14. Vector plots of particle displacement field. Particle displacement fields imposed by device under -30pm motion on the surrounding agarose. Scale of vector magnitude ranges from 0-30pm. Left to right: Uncoated, PEG-2000 coating, PEG-8000 coating 22 Figure 15. Particle displacement field vector plot overlays. Images of the particle displacement fields associated with uncoated (A), PEG-2000 coated (B), and PEG-8000 coated (C) overlaid on images of the devices immersed in the agarose. 23 Magnitude,f Magnitue 'r Vtor tm) V-1"or (W") 30 Figure 16. Particle displacement field cross sections. Cross sections of the particle displacement fields near the tip of the uncoated (left) and PEG-8000 coated (right) devices. Magnitude of the particle displacement vector is plotted. The red shaded area is the actual device. for The coated device is much larger because of the coating. The particle displacements are lower sample. the of modulus the PEG-8000 coated device due to the lower 2000Mw Magnitude of Vector (pm) 0! 25 90 20 9 9 15 Sg 9 9 9 999 *9 9 69 -PI 10 I 500 r 1000 y-position (pmn) 1500 Figure 17. Particle displacement field cross section of PEG-2000 coated device. Cross section of the particle displacement fields near the tip of the PEG-2000 coated device. This coated device only has a significant amount of coating on the bottom (corresponds to the left side) and the agarose on that side has a reduced particle displacement when compared to the nearly uncoated top (right in this image). 24 Displacment at Surface 40 35 30 25 20 S R~. 10 10 0 8000 Mw Uncoated 2000 Mw uncoated side 2000 Mw Coated side Figure 18. Displacement at Surface. Comparison of particle displacement near the surface of the device. For the PEG 2000 coating the two sides of the device were analyzed separately due to the loss of hydrogel coating on one side. Conclusions The use of PEG hydrogel coatings on glass brain implant devices reduces the strain field imposed by those devices on tissue due to brain micromotion. The lower modulus of the hydrogel coating acts as a remedy to the mechanical mismatch between the high modulus glass (~69 GPa) and the low modulus brain tissue (5 kPa). The moduli of these coating can be controlled to an extent using varying concentration of PEG in solution before gelation. It is possible that the modulus can also be controlled by varying the degree of swelling, or by varying the chain lengths to a much higher degree. Thickness of the gel may also be a factor in the moduli of the gel if the gels are thin enough that there are still residual effects of the high modulus glass even at the surface of the gel. 25 The reduction in strain field should reduce the extent of glial scarring near the implant area of the device. In effect, the addition of PEG hydrogel coatings should improve the effectiveness and longevity of the device. More work needs to be done to understand the effects of the act of implantation on the hydrogel coating to prevent shearing and the effect of gel swelling on the device. 26 References 1. DeLong, M. R. & Wichmann, T. Circuits and circuit disorders of the basal ganglia. Arch. Neurol. 64, 20-24 (2007). 2. Marsh, R., Maia, T. V & Peterson, B. S. Functional disturbances within frontostriatal circuits across multiple childhood psychopathologies. Am. J.Psychiatry 166, 664-674 (2009). 3. Amemori, K. & Graybiel, A. M. Localized microstimulation of primate pregenual induces negative decision-making. Nat. Neurosci. 15, 776-785 (2012). 4. Ponce, F. A. & Lozano, A. M. in Prog. Brain Res. 311-324 (2010). 5. Gradinaru, V., Mogri, M., Thompson, K. R., Henderson, J. M. & Deisseroth, K. Optical deconstruction of parkinsonian neural circuitry. Science 324, 354-359 (2009). 6. Krack, P., Hariz, M. I., Baunez, C., Guridi, J. & Obeso, J. A. Deep brain stimulation: From neurology to psychiatry? Trends Neurosci. 33, 474-484 (2010). 7. Polikov, V. S., Tresco, P. a & Reichert, W. M. Response of brain tissue to chronically implanted neural electrodes. J. Neurosci. Methods 148, 1-18 (2005). 8. Lee, H., Bellamkonda, R. V, Sun, W. & Levenston, M. E. Biomechanical analysis of silicon microelectrode-induced strain in the brain. J. Neural Eng. 2, 81-89 (2005). 9. Foley, C. P., Nishimura, N., Neeves, K. B., Schaffer, C. B. & Olbricht, W. L. Flexible microfluidic devices supported by biodegradable insertion scaffolds for convection-enhanced neural drug delivery. Biomed. Microdevices 11, 915-924 (2009). 10. Szarowski, D. 1-1. et al. Brain responses to micro-machined silicon devices. Brain Res. 983, 23-35 (2003). IL. Rousche, P. J. & Normann, R. A. Chronic recording capability of the utah intracortical electrode array in cat sensory cortex. J. Neurosci. Methods 82, 1-15 (1998). 12. Kipke, D. R., Vetter, R. J., Williams, J. C. & Hetke, J. F. Silicon-substrate intracortical microelectrode arrays for long-term recording of neuronal spike activity in cerebral cortex. IEEE Trans. Neural Syst. Rehabil. Eng. 11, 151-155 (2003). 13. Butson, C. R., Maks, C. B. & McIntyre, C. C. Sources and effects of electrode impedance during deep brain stimulation. Clin. Neurophysiol. 117, 447-454 (2006). 14. Seymour, J. P. & Kipke, D. R. Neural probe design for reduced tissue encapsulation in CNS. Biomaterials 28, 3594-3607 (2007). 15. Peppas, N. a., Hilt, J. Z., Khademhosseini, A., Langer, R. & Peppas, B. N. A. [lydrogels in biology and medicine: From molecular principles to bionanotechnology. Adv. Mater. 18, 1345-1360 (2006). 16. Peppas, N. A. Hydrogels and drug delivery. Curr. Opin. Colloid Interjace Sci. 2, 531-537 (1997). cingulate cortex 27 17. Kim, D. H., Wiler, J. A., Anderson, D. J., Kipke, D. R. & Martin, D. C. Conducting polymers on hydrogel-coated neural electrode provide sensitive neural recordings in auditory cortex. Acta Biomater. 6, 57-62 (2010). 18. Kim, D.-H., Abidian, M. & Martin, D. C. Conducting polymers grown in hydrogel scaffolds coated on neural prosthetic devices. J. Biomed. Mater. Res. A 71, 577-585 (2004). 19. Eng, L. F. Glial fibrillary acidic protein (GFAP): the major protein of glial intermediate filaments in differentiated astrocytes. J. Neuroimmunol. 8, 203-214 (1985). 20. Schmidt, S., Horch, K. & Nornann, R. Biocompatibility of silicon-based electrode arrays implanted in feline cortical tissue. J.Biomed. Mater. Res. 27, 1393-1399 (1993). 21. Sykovi, E., Vargovi, L., Prokopovi, S. & Simonovi, Z. Glial swelling and astrogliosis produce diffusion barriers in the rat spinal cord. Glia 25, 56-70 (1999). 22. Ridet, J. L., Malhotra, S. K., Privat, A. & Gage, F. H. Reactive astrocytes: Cellular and molecular cues to biological function. Trends Neurosci. 20, 570-577 (1997). 23. Turner, J. N. et al. Cerebral astrocyte response to micromachined silicon implants. Exp. Neurol. 156, 33-49 (1999). 24. Farra, R. et al. First-in-Human Testing of a Wirelessly Controlled Drug Delivery Microchip. Sci. Transl. Med. 4, 122ra21-122ra21 (2012). 25. Voskerician, G., Liu, C.-C. L. C.-C. & Anderson, J. M. Electrochemical characterization and in vivo biocompatibility of a thick-film printed sensor for continuous in vivo monitoring. IEEE Sens. J. 5, (2005). 26. Anderson, J. M., Rodriguez, A. & Chang, D. T. Foreign body reaction to biomaterials. Semin. Immunol. 20, 86-100 (2008). 27. Prasad, A. et al. Comprehensive characterization and failure modes of tungsten microwire arrays in chronic neural implants. J. Neural Eng. 9, 056015 (2012). 28. Rolls, A., Shechter, R. & Schwartz, M. The bright side of the glial scar in CNS repair. Nat. Rev. Neurosci. 10, 235-241 (2009). 29. Silver, J. & Miller, J. H. Regeneration beyond the glial scar. Nat. Rev. Neurosci. 5, 146-156 (2004). 30. Grill, W. M. in Indwelling NeuralImplant. Strateg. Contend. with Vivo Environ. 1-14 (2008). doi:NBK3931 [bookaccession] 31. Shannon, R. V. A model of safe levels for electrical stimulation. IEEE Trans. Biomed. Eng. 39, 424-426 (1992). 32. Vorisek, I., Hijek, M., Tintera, J., Nicolay, K. & Sykovi, E. Water ADC, extracellular space volume, and tortuosity in the rat cortex after traumatic injury. Magn. Reson. Med. 48, 994-1003 (2002). 28 33. Roitbak, T. & Sykovi, E. Diffusion barriers evoked in the rat cortex by reactive astrogliosis. Glia 28, 40-48 (1999). 34. Potter, K. A., Buck, A. C., Self, W. K. & Capadona, J. R. Stab injury and device implantation within the brain results in inversely multiphasic neuroinflammatory and neurodegenerative responses. J Neural Eng. 9, 046020 (2012). 35. Kolarcik, C. L. et al. In vivo effects of LI coating on inflammation and neuronal health at the electrode-tissue interface in rat spinal cord and dorsal root ganglion. Acta Biomater. 8, 3561-3575 (2012). 36. Sham, W. et al. Controlling cellular reactive responses around neural prosthetic devices using peripheral and local intervention strategies. IEEE Trans. Neural Syst. Rehabil. Eng. 11, 186-188 (2003). 37. Gilletti, A. & Muthuswamy, J. Brain micromotion around implants in the rodent somatosensory cortex. J. Neural Eng. 3, 189-95 (2006). 38. Fee, M. S. Active stabilization of electrodes for intracellular recording in awake behaving animals. Neuron 27, 461-468 (2000). 39. Karumbaiah, L. et al. Relationship between intracortical electrode design and chronic recording function. Biomaterials34, 8061-8074 (2013). 40. Biran, R., Martin, D. C. & Tresco, P. A. The brain tissue response to implanted silicon microelectrode arrays is increased when the device is tethered to the skull. J Biomed. Mater. Res. A 82, 169-178 (2007). 41. Lin-Gibson, S. et al. Synthesis and characterization of PEG dimethacrylates and their hydrogels. Biomacromolecules 5, 1280-7 (2004). 42. Van Lehn, R. & Alexander-katz, A. Suggested reading. 1-7 (2012). 43. Subbaroyan, J., Martin, D. C. & Kipke, D. R. A finite-element model of the mechanical effects of implantable microelectrodes in the cerebral cortex. J. Neural Eng. 2, 103-113 (2005). 44. Revzin, a et al. Fabrication of poly(ethylene glycol) hydrogel microstructures using photolithography. Langnuir 17, 5440-7 (2001). 45. Brzoska, J. B., Azouz, 1. Ben & Rondelez, F. Silanization of Solid Substrates: A Step Toward Reproducibility. Langnuir 10, 4367-4373 (1994). 46. Beamish, J. a, Zhu, J., Kottke-Marchant, K. & Marchant, R. E. The effects of monoacrylated poly(ethylene glycol) on the properties of poly(ethylene glycol) diacrylate hydrogels used for tissue engineering. J. Biomed. Mater. Res. A 92, 441-50 (2010). 47. Lin, D. C., Dimitriadis, E. K. & lorkay, F. Robust strategies for automated AFM force curve analysis--I. Non-adhesive indentation of soft, inhomogeneous materials. J. Biomech. Eng. 129, 430-40 (2007). 48. Hafner, J. H., Cheung, C. L., Woolley, a T. & Lieber, C. M. Structural and functional imaging with carbon nanotube AFM probes. Prog. Biophys. Mol. Biol. 77, 73-110 (2001). 29 49. Callister, W. D. Materials Science and Engineering:An Introduction. (John Wiley & Sons, 2007). 50. Buschow, K. H. J. Encylopedia of Materials:Science and Technology. (Elsevier, 2001). 30