EGR 115 – Fall 2013 0. Defining Roughness This is to be completed individually. In the NanoRoughness_AnswerSheet.docx file, answer the following questions: a. What procedure might you use to measure the roughness of the pavement on a road? b. Give an example (other than road pavement) of something for which degree of roughness matters. o For your example, why does the degree of roughness matter? o How might you measure the roughness (or lack of roughness) of this object? c. How do you define roughness? Does the definition of roughness change when you think about different objects for which roughness might matter? Why or why not? 1. Atomic Force Microscopy Background This is to be completed individually. Read the following explanation about Atomic Force Microscopy and IN YOUR OWN WORDS answer the following questions in the answer sheet document. a. What are the three modes of the AFM, and what are the advantages/disadvantages of each? b. What is the AFM resolution limit? c. What causes the resolution limit? Atomic Force Microscopy (AFM) 1 The primary purpose of Atomic Force Microscopy (AFM) is to quantitatively measure nanoscale surface features and forces with a nominal 0.1 nm lateral and 0.05 nm vertical resolution on all types of samples. AFM works essentially like an old-school record player the kind used to play music recorded on vinyl. A high-tech version of the old-school record player stylus moves over a surface of interest and the behavior of the arm supporting the stylus is translated into measurements. In AFM, the stylus is called a cantilever tip. The probe is an etched silicon or silicon nitride chip with a cantilever extending from the chip and a sharply etched cone, known as the tip, located on the underside of the cantilever. As the cantilever tip approaches the surface, it experiences an initial attractive force 1 References: Phil Russell, Dale Batchelor, John T. Thornton “SEM and AFM: Complementary Techniques for High Resolution Surface Investigations” 2004, AN46, Rev A1, Veeco Instruments, Santa Barbara, CA. EGR 115 – Fall 2013 (polarization forces), which is replaced by a repulsive force as the tip makes physical contact with the specimen. A laser focused on the backside of the cantilever monitors the displacement of the probe and provides feedback as the probe scans across the sample surface. The probe is perpetually scanned across the sample surface either in contact with the surface (Contact Mode), at a constant distance (Noncontact Mode), or while the cantilever is oscillating at a defined frequency (Tapping Mode). These modes are demonstrated in Figure 1. All three modes map the topography of the surface although each has limitations and advantages. Contact Mode can directly measure surface forces, opening the door to calculating adhesion and friction forces at the nanoscale, but can damage sample surface. Tapping Mode has the lowest surface forces and can provide detailed information about the difference in surface phase behavior, thus allowing biological and soft polymer samples to be characterized. AFM can be used to image surfaces with atomic resolution as well as surface forces at nano-Newton scales. The shape and radius of the cantilever tip limits the resolution of the topography images captured from AFM. A sharper tip follows the hills and valleys of the surface more closely, leading to better resolution than scanning with a blunter tip. Similar to feeling with your fingertip, a sharp tip can response to a change in surface height, while a blunter tip, similar to your elbow, overestimates large differences and neglects smaller differences (demonstrated in Figure 2). Depending on the AFM design, piezo scanners either translate (move) the sample under the cantilever or the cantilever over the sample. As the cantilever tip scans the surface, the cantilever arm responses to differences in sample height by deflecting the laser center on the backside. The difference in deflection is measured and translated into height data, thereby constructing a three-dimensional topographical map of the surface by plotting the local sample height versus horizontal probe tip position. Thus, AFM images are resolved in three dimensions and the difference in surface features can be quantified. A B C Figure 1: Three modes of the AFM: (A) contact, (B) non-contact, and (C) tapping. The AFM outputs are shown below each diagram. The black arm represents the cantilever beam, and the triangle represents the probe tip. EGR 115 – Fall 2013 Figure 2: Interaction between a sharp tip and a surface feature of a sample, showing the resolution limit of the AFM. (The top, thin, line is the output of the AFM. Note the shallower depth of the same well for the wider tip.) Comparison of AFM to Other Common Techniques: Scanning Electron Microscopy images the sample using electrons reflected and refracted from the surface layer. Samples must be coated in a conductive layer (typically gold) and placed in a vacuum chamber (typically 10-6 torr). SEM has similar lateral resolution of images (0.7nm) but views surfaces on a focus plane, thereby limiting the depth of focus in a single image. Direct height measurements of surface features can be taken similar to measuring distances on a map but topographical relief in images is similar to pictures (not quantifiable). The shading is due to differences in observed reflected light, not direct height measurements. Unlike AFM, SEM cannot be used to quantify the height of surface structures or obtain information related to surface forces. Optical Microscopy images a sample surface by observing the reflected and refracted light directed through a series of lenses. The lateral resolution of optical microscopy is significantly higher than SEM and AFM. Optical microscopy has a limited focus depth since the lenses have a focal point, not a focal plane. Images of samples with large height steps often have areas out of focus due to the inability to bring all heights into focus simultaneously. By comparison, AFM provides unambiguous measurement of step heights, independent of reflectivity differences between materials. 2. Nano Roughness This is to be completed individually. 1. Read the company profile and the memo from Kerry Prior that follows. 2. On your answer sheet, answer the following questions. a. List as many stakeholders as you can think of who may be impacted by the deliverable your team has been asked to create. For each stakeholder, explain the relationship between the stakeholder, the problem, and the deliverable. b. Your solution will be implemented in the context described here and potentially in other contexts. Describe issues (minimum five) that might arise for stakeholders when your generalizable solution is implemented. EGR 115 – Fall 2013 c. Consider your list of stakeholders. Who is the direct user of the deliverable your team is being asked to create? d. In a few sentences and in your own words, what does the direct user need? (Remember to describe the deliverable, its function, the criteria for success, and the constraints.) e. Consider the immediate problem as described and the sample data provided. Describe at least two ideas you have for why this problem might be complex to solve. Company Profile – Liguore Laboratories Liguore Laboratories is an emerging technology company founded in 1996 to develop nanostructured materials that improve performance and extend the life of coated orthopedic and biomedical implants. The coating of orthopedic implants, such as joint replacements, is undertaken with the aim of either increasing the wear resistance of the implant materials or providing an implant surface that increases the biocompatibility of the implant with the surrounding host bone. This increase in biocompatibility leads to formation of new bone around the implant resulting in better fixation and improved long-term performance of the replacement joint. Our company produces coatings for biomedical devices such as artery stents, bone screws, fixation devices, and bone spacers. Liguore Laboratories utilizes surface coating techniques to apply a full range of bioactive coatings to orthopedic and biomedical implants manufactured by several global manufacturers. The coatings include titanium, hydroxyapatite, alumina/titania, gold, calcium phosphate, and other alloys. Our company has met and exceeded all industry and health standards for the United States and Europe. One of our more recent developments is the use of gold to coat artery stents. The Liguore Laboratories materials research team found that gold, when heated, makes a smooth surface coating for implants. The stents coated with lower roughness gold possess more biocompatibility than stents coated with stainless steel. Liguore Laboratories has assembled a talented group of scientists and engineers who possess an in-depth understanding of the processes available for synthesizing the end product. They consult regularly with leading biomaterials scientists, cell biologists, and clinical researchers within the global community to develop innovative products that meet the clinicians' needs. Liguore Laboratories is on the cutting edge of technology in the biomedical coatings industry. Our mission is to create medical device coatings that provide performance and durability. EGR 115 – Fall 2013 INTEROFFICE MEMO: LIGUORE LABS TO: NANOSURFACE ENGINEERING TEAM FROM: KERRY PRIOR, VICE PRESIDENT OF RESEARCH RE: SURFACE ROUGHNESS Liguore Labs is very interested in the innovations of biomedical science. New research pertaining to coatings for artificial hip replacements could represent a new venture for our company. Recently, a physicist from University of Alabama, Birmingham named Dr. Yogesh Vohra accidentally produced smooth diamond. When making synthetic diamond crystals in a laboratory, the gas reactor sprang a small leak and let air into the mixture. Nitrogen from the air reacted with the carbon of the diamond. The array of diamond created was smooth and adhered very easily to metal. Because diamond is durable, it makes a very good candidate for coating artificial hip replacements. The current coatings wear down or loosen from constant use after about 10 years, which could mean more surgery for the recipient. The diamond coating is projected to last around 40 years, which would improve the comfort and health of the patient. Liguore Laboratories would like to expand our product line to include diamond coatings for hip joints. The research laboratory is working on replicating the smooth diamond coating. In order for our materials research team to know whether their production process is working (achieving the desired level of smoothness), they need a quick and easy-to-use procedure to quantify the roughness of the nanoscale diamond coatings produced in the lab. Since we have experience with gold coatings and have many AFM images and data sets available, your team can use these to develop a procedure to quantify the roughness of new coatings. Your team will be provided with three atomic force microscope (AFM) images and associated data for gold coatings that we have produced in our artery stent research lab. These images and data are described in the attached Background Information attached. Your team needs to create a repeatable procedure using these images and data as a reference to quantify the roughness at the nanoscale. Your team also needs to apply your procedure to the AFM gold images and data. With this procedure in place, our materials research team will be able to quickly quantify the roughness of the diamond coating samples as they are produced. In a memo to my attention, please include your team’s procedure for quantifying roughness of the nanoscale material using the AFM images and data. For this first iteration, provide results of applying your procedure to the AFM gold image and data Sample C only. Please be sure to include your team’s reasoning for the each step, heuristic (i.e. rule), or consideration in your team’s procedure. Thank you for your team’s efforts in this endeavor. The expansion of our product line is an important venture for Liguore Laboratories. I appreciate your prompt attention to this assignment. Kerry Prior Attached: Background Information Background Information: The two images on this page are images of smooth diamond from Dr. Vohra’s lab. Figure 1a is a top-view image of the diamond. Figure 1b is a 3-dimensional side-view EGR 115 – Fall 2013 of the same sample. The color bar on the right indicates the height of the diamond surface. Remember that: μm stands for micrometers (1 μm = 10-6 m) nm stands for nanometers (1 nm = 10-9 m) Å stands for Angstroms (1 Å = 10-10 m) Figure 1a. Top-view AFM image of smooth diamond. Figure 1b. Three-dimensional AFM image of smooth diamond. EGR 115 – Fall 2013 AFM Images: (AFM data courtesy of Purdue Nanoscale Physics Lab) The three images below (Samples A, B, and C) are top-view images of gold that are provided for use in developing your team’s procedure for quantifying roughness. The colorbar on the right indicates the height of the gold surface. These images are generated from AFM data which consists of the cantilever’s (X,Y) location and local height as the cantilever is drawn over the surface of the sample. For instance, the first few and the last few data points for Sample A would be: WSxM file copyright Nanotec Electronica WSxM ASCII XYZ file X[µm] Y[µm] Z[Å] 0.000000 0.011742 0.023483 …. ….. 5.976517 5.988258 6.000000 0.000000 0.000000 0.000000 675.345 671.311 667.278 6.000000 6.000000 6.000000 332.301 343.649 372.94 These height values can be arranged into an array and then translated into color values (in this case grayscale values) so that the data can be visualized. The total number of (X,Y,height) data points to generate a complete image can be quite large - for Sample A it is 262,146. Your team is provided with a slice of each of the three data sets so that you do not have to handle such large data sets (which could crash your computer) but still get give you a sense of the data. Three AFM data files are available for your team to use to as a reference when developing your procedure. The filenames are indicated with the images below. In the Excel file, you will find two worksheet tabs: goldSampleX_view100%: is a slice of the height data arranged in an array according to the (X,Y) locations (the X,Y locations are noted across row1,columnA, respectively, in µm). Cells in which the height data are stored (in Å = angstrom) are conditionally formatted for grayscaling so that the image appears when the spreadsheet is zoomed to 10%. This sheet is set to view at 100% so that you can see and use the height values. goldSampleX_view10%: is identical to goldSampleX_view100%, but the view is set to 10% so that you can view the image slice. Note that the image slice constructed in Excel is the bottom portion of each of the images below rotated 90 degrees. EGR 115 – Fall 2013 Sample A goldSampleA.xlsx Sample B goldsampleB.xlsx EGR 115 – Fall 2013 Sample C goldSampleC.xlsx